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Method of preparing metal organic framework materials through conversion method

A technology of metal-organic framework and transformation method, which is applied in the field of preparation of metal-organic framework materials, can solve the problems that hinder the development of high-stability MOF, and achieve the effect of easy amplification, wide application and excellent performance

Active Publication Date: 2016-02-03
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Complex and harsh synthetic conditions will greatly hinder the development of such highly stable MOFs

Method used

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  • Method of preparing metal organic framework materials through conversion method
  • Method of preparing metal organic framework materials through conversion method
  • Method of preparing metal organic framework materials through conversion method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1 Preparation of CuBDC, MIL-53 and UIO-66 by MOF-5 Conversion of Hydrothermal Synthesis

[0030] (1) Preparation of MOF-5 by hydrothermal method: Weigh 1.73g of zinc nitrate hexahydrate and 0.32g of terephthalic acid and dissolve them in 20mL of NN′-dimethylformamide to obtain two clarified metal-organic framework precursors solution, the two metal-organic framework precursor solutions were mixed and transferred to a hydrothermal kettle, heat-treated at 110°C for 18h, then the hydrothermal kettle was placed at room temperature to cool naturally, and then centrifuged at 5000 rpm, The obtained MOF-5 particles were washed successively with NN′-dimethylformamide (20 mL×2), methanol (20 mL×2), and finally dried at 80° C. to obtain 0.853 g of MOF-5 particles.

[0031] (2) Conversion and preparation of CuBDC: Weigh 0.5g of copper nitrate trihydrate and dissolve it in 20mL of ethanol to obtain a copper nitrate solution; weigh 0.1g of MOF-5 prepared in step (1), and plac...

Embodiment 2

[0041] Example 2 Preparation of CuBDC, MIL-53 and UIO-66 by conversion of MOF-5 synthesized by stirring

[0042](1) Preparation of MOF-5 by stirring method: Weigh 1.21g of zinc nitrate hexahydrate and dissolve it in 100mLNN'-dimethylformamide, then add 0.34g of terephthalic acid, and then add 1.6g of triethylamine under stirring And reacted for 2 hours, then centrifuged at 5000 rpm to obtain MOF-5 particles, washed with NN'-dimethylformamide (20mL×2) and methanol (20mL×2) in sequence, and finally heated at 80°C Dry to obtain 0.096g of MOF-5 particles.

[0043] The process of converting and preparing CuBDC, MIL-53 and UIO-66 is the same as that of Example 1.

Embodiment 3

[0044] Example 3 Preparation of MIL-53 and UIO-66 by CuBDC Conversion

[0045] (1) Preparation of CuBDC: Weigh 0.93g of copper nitrate trihydrate and 0.66g of terephthalic acid and dissolve them in 50mL of NN'-dimethylformamide respectively to obtain clear solutions of two metal-organic framework precursors. The metal-organic framework precursor solution was mixed and transferred to a hydrothermal kettle, heat-treated at 110 °C for 24 h, then the hydrothermal kettle was placed at room temperature to cool naturally, and then centrifuged at 5000 rpm to obtain CuBDC particles, followed by Wash with NN′-dimethylformamide (40 mL×2) and methanol (40 mL×2), and finally dry at 80° C. to obtain 1.28 g of CuBDC particles.

[0046] (2) Conversion and preparation of MIL-53: 4 g of ferric nitrate was weighed and dissolved in 20 mL of ethanol to obtain a ferric nitrate solution. Weigh 0.1 g of CuBDC prepared in step (1), place it in the prepared ferric nitrate solution, react at 20° C. for...

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Abstract

The invention provides a method of preparing metal organic framework materials through a conversion method. According to the method, firstly, metal salt is dissolved in organic solvent to obtain metal salt solution with the concentration between 0.0025 g / mL and 0.2 g / mL; secondly, the metal organic framework material A is placed in the metal salt solution at the reaction temperature between 20 DEG C and the boiling point temperature of the organic solvent in the metal salt solution for the reaction time of 2-48h, and aftertreatment is conducted after reaction is over to obtain the metal organic framework material B. Mild conditions are adopted for converted synthesis of a metal organic framework which generally requires strict synthesis conditions; traditional high-temperature hydrothermal synthesis conditions are abandoned, operation is simple, and amplification is easy; the synthesized metal organic framework materials are wide in usage, capable of being used for adsorption and catalytic degradation and excellent in performance.

Description

(1) Technical field [0001] The invention relates to a method for preparing a metal organic framework material, in particular to a method for directly converting an easy-to-synthesize metal-organic framework material into a generally difficult-to-synthesize metal-organic framework material. (2) Background technology [0002] A new type of porous metal-organic framework material has been developed and synthesized in large quantities because of its huge specific surface area, adjustable pore structure, excellent stability, and gas selective adsorption. However, there are also great differences in the synthesis methods of different metal-organic frameworks. HKUST-1, MOF-5, etc., as metal-organic frameworks developed in the early stage, are widely used in separation, catalysis, adsorption and other fields, and these types of MOF materials have been prepared on a large scale. In general, however, these kinds of MOFs are less stable. Metal-organic framework materials with trivale...

Claims

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Application Information

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IPC IPC(8): C07F1/08C07F15/02C07F7/00
Inventor 张国亮李万斌
Owner ZHEJIANG UNIV OF TECH
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