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A template-free, solvent-free, rapid and efficient method for synthesizing metal-organic framework uio-66(zr)

A metal-organic framework and template-free technology is used in the field of template-free, solvent-free, fast and efficient synthesis of metal-organic framework materials UiO-66(Zr), and the effect of shortening the crystallization time is achieved.

Active Publication Date: 2021-11-19
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the shortcomings of the existing UiO-66(Zr) synthesis method, the present invention provides a template-free, solvent-free, fast and efficient method for synthesizing metal-organic framework material UiO-66(Zr)

Method used

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  • A template-free, solvent-free, rapid and efficient method for synthesizing metal-organic framework uio-66(zr)
  • A template-free, solvent-free, rapid and efficient method for synthesizing metal-organic framework uio-66(zr)
  • A template-free, solvent-free, rapid and efficient method for synthesizing metal-organic framework uio-66(zr)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In this example, the metal-organic framework material UiO-66(Zr) was synthesized according to the following steps:

[0025] 1. Analytical pure zirconium oxychloride octahydrate (ZrOCl 2 ·8H 2 O) mixed with terephthalic acid in a molar ratio of 1:1, ground at room temperature for 20 min, then moved into a stainless steel reaction kettle with polytetrafluoroethylene lining, and crystallized at 100° C. for 24 h.

[0026] 2. After the reactor is cooled, take out the solid.

[0027] 3. Wash with absolute ethanol at 60°C for 8 hours, separate the solid by filtration, and dry at 100°C.

[0028] 4. After repeating step 3 2 times, UiO-66 powder is finally obtained.

Embodiment 2

[0030] In this example, the metal-organic framework material UiO-66(Zr) was synthesized according to the following steps:

[0031] 1. Analytical pure zirconium oxychloride octahydrate (ZrOCl 2 ·8H 2 O) mixed with terephthalic acid in a molar ratio of 1:1, ground for 20 minutes at room temperature, then moved into a stainless steel reaction kettle with polytetrafluoroethylene lining, and crystallized at 120°C for 24 hours.

[0032] 2. After the reactor is cooled, take out the solid.

[0033] 3. Wash with N,N-dimethylamide at 60°C for 8 hours, separate the solid by filtration, and dry at 100°C.

[0034] 4. After repeating step 3 2 times, UiO-66 powder is finally obtained.

Embodiment 3

[0036] In this example, the metal-organic framework material UiO-66(Zr) was synthesized according to the following steps:

[0037] 1. Analytical pure zirconium oxychloride octahydrate (ZrOCl 2 ·8H 2 O) mixed with terephthalic acid in a molar ratio of 1:1, ground for 20 minutes at room temperature, then moved into a stainless steel reactor with a polytetrafluoroethylene liner, and crystallized at 140° C. for 24 hours.

[0038] 2. After the reactor is cooled, take out the solid.

[0039] 3. Wash with absolute ethanol at 60°C for 8 hours, separate the solid by filtration, and dry at 100°C.

[0040] 4. After repeating step 3 2 times, UiO-66 powder is finally obtained.

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Abstract

The invention discloses a method for quickly and efficiently synthesizing a metal-organic framework material UiO-66(Zr) without a template agent and without a solvent. The method comprises the following steps: 1. mixing an inorganic zirconium salt with terephthalic acid, Grinding, then moving into a stainless steel reaction kettle with polytetrafluoroethylene lining for crystallization; 2. After the reaction kettle is cooled, take out the solid; 3. Wash with an organic solvent, filter and separate the solid, and dry; 4. After repeating step 3 for 2-4 times, UiO-66(Zr) powder is finally obtained. The present invention has the following advantages: 1. The method of the present invention can obtain crystals with a UiO-66 skeleton structure; 2. The method of the present invention can greatly shorten the crystallization time; 3. The method of the present invention can adjust the synthesis parameters, UiO‑66 crystals with different surface areas were obtained.

Description

technical field [0001] The invention is the improvement and optimization of the synthesis method of metal organic framework material UiO-66(Zr). Background technique [0002] As a new type of porous material, metal-organic frameworks (MOFs) are widely used in sensing, gas adsorption, separation, storage and transportation, catalysis, etc. It has broad application prospects in the fields of encapsulation and release of targeted drugs. Among them, UiO-66 not only has the above advantages, but also has good chemical, physical and thermal stability, and has greater potential applications. [0003] UiO-66(Zr) was first synthesized by K.P. Lillerud's team in 2008 and published in the Journal of the American Chemical Society. UiO-66(Zr) is a cage structure formed by zirconium metal element as the central metal ion and terephthalic acid (BDC) as the organic ligand. Zirconium elements are connected with oxygen atoms in an eight-coordinated manner to form a twelve-connected zirconi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 孙印勇叶干
Owner HARBIN INST OF TECH