Method for preparing MOF-5

A MOF-5, terephthalic acid technology, applied in the direction of zinc organic compounds, can solve the problems of high equipment requirements and difficult to popularize, and achieve the effects of good particle consistency, simple operation and good thermal stability

Inactive Publication Date: 2013-10-02
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Later, some researchers prepared MOF-5 by microwave heating, pre-seed and electrochemical methods. The Langmuir specific surface area of ​​the prepared MOF-5 was up to 2798m 2 / g, but these methods require too much equipment and are difficult to popularize

Method used

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  • Method for preparing MOF-5
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  • Method for preparing MOF-5

Examples

Experimental program
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Embodiment 1

[0024] Weigh 3.06g zinc chloride and dissolve it in 50mL DMF to make solution A, weigh 2.5g terephthalic acid and dissolve it in 100mL DMF to make solution B, add 3mL triethylamine to B, mix well and heat B To 120°C, solution A was added dropwise to solution B at a rate of 120 μL / min, and the stirring rate was maintained at 400 r / min. After 7 hours, 3 g of MOF-5 was obtained, and the pH of the solution was 4 during the reaction. The Langmuir specific surface area of ​​MOF-5 is 1563m 2 / g, its decomposition temperature by thermogravimetric analysis is 400°C.

Embodiment 2

[0028] Weigh 1.8g zinc acetate and dissolve it in 1000mL NMP to make solution A, weigh 0.5g terephthalic acid and dissolve it in 1000mL NMP to make solution B, add 3mL deionized water to B, mix well and heat B to 50 °C, solution A was added dropwise to solution B at a rate of 1.5 mL / min without stirring, and 0.5 g MOF-5 was obtained after 12 hours, and the pH value of the solution during the reaction was 4.5. The Langmuir specific surface area of ​​MOF-5 is 2522m 2 / g, its decomposition temperature by thermogravimetric analysis is 400°C.

Embodiment 3

[0032] Weigh 5.65g zinc nitrate hexahydrate and dissolve it in 100mL DEF to make solution A, weigh 1.33g terephthalic acid and dissolve it in 100mL DEF to make solution B, heat A to 105°C, and drop B at 70μL / min Add it into solution A, keep the stirring speed at 200r / min, and obtain 1.9g MOF-5 after 24 hours, and the pH value of the solution is 5 during the reaction. Langmuir specific surface area is 2700m 2 / g, its decomposition temperature by thermogravimetric analysis is 400°C.

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Abstract

The invention discloses a method for preparing MOF-5 and belongs to the technical field of preparation of metal framework materials. Zinc sources and terephthalic acid are dissolved in solvents separately. One solution is heated, and the other solution is added into the heated solution dropwise to prepare MOF-5 by a solvothermal method. The method not only utilizes existing devices, but also controls the degree of supersaturation of reaction solutions at a low level without consuming more solvents to prepare MOF-5 with good granule consistency, high specific surface area and good thermostability. The method reduces consumption of solvents, and has loose facility requests and simple operations, and MOF-5 can be prepared economically and effectively.

Description

technical field [0001] The invention relates to a method for preparing MOF-5, which belongs to the technical field of metal organic framework material preparation. Background technique [0002] In the crystal growth process, the main factors affecting its secondary nucleation are temperature, stirring, supersaturation, impurities, and crystal size. Supersaturation is one of the most important factors affecting secondary nucleation, and the regulation of supersaturation There are many methods, one of which is to adjust the concentration of the reaction solution. [0003] Metal-organic framework (MOF) is a topological porous polymer material formed by the combination of metal ions and organic ligands through coordination bonds. It has the characteristics of more unsaturated metal sites, high specific surface area and high thermal stability. It can be used in various fields such as gas separation, gas storage, chemical catalysis, chemical sensing and drug release. Among them...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/06
Inventor 刘晋李劼韩鹏飞
Owner CENT SOUTH UNIV
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