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Metal organic framework material HKUST-1 and preparation method thereof

A metal-organic framework, HKUST-1 technology, applied in the field of metal-organic framework material HKUST-1 and its preparation, can solve the problems of incomplete crystal form of metal-organic framework materials, inability to transform products in time, poor hydrothermal stability, etc., to achieve Effects of shortening the crystal nucleus growth period, improving surface free energy, and increasing yield

Active Publication Date: 2018-03-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above-mentioned ultrasonic synthesis method can synthesize metal-organic framework material HKUST-1 quickly and with high yield, but because the synthesis speed is too fast, the product cannot be transformed into a perfect crystal form in time, and even does not have the unique crystal form of metal-organic framework materials; moreover, Ultrasound produces strong shock waves, and the huge shearing and dispersing effects caused by micro jets destroy larger nanoparticles and further damage the crystals, eventually leading to incomplete crystal forms of metal-organic framework materials and poor hydrothermal stability. question

Method used

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  • Metal organic framework material HKUST-1 and preparation method thereof
  • Metal organic framework material HKUST-1 and preparation method thereof
  • Metal organic framework material HKUST-1 and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0035] Weigh 0.6g of HKUST-1 seed crystal, add it to 20mL of ethanol, and sonicate at 300W for 20min to prepare mixed slurry A; weigh 21g of copper nitrate trihydrate and 10.08g of trimesic acid, add it to 600mL of ethanol In a mixed solution with DMF, including 300mL ethanol and 300mL DMF, prepare solution B; mix the mixed slurry A and solution B, stir the solution at 200rpm at 75°C for reaction and maintain it for 20h, filter the reaction solution, soak and wash with ethanol The reaction product was twice, ultrasonicated at a power of 300W for 5min during the soaking process, and the washed product was dried at 100°C for 20h to obtain the final product, which was labeled as metal organic framework material A.

Embodiment 2

[0037]Weigh 0.6g of HKUST-1 seed crystal, add it to 20mL of ethanol, and sonicate at 300W for 20min to prepare mixed slurry A; weigh 21g of copper nitrate trihydrate and 10.08g of trimesic acid, add it to 600mL of ethanol In a mixed solution with DMF, in which ethanol 180mL, DMF 420mL, prepare solution B; mix the mixed slurry A and solution B, stir the solution at 78°C at 250rpm for reaction and maintain for 20h, filter the reaction solution, soak and wash with ethanol The product was reacted twice, and the washed product was dried at 150° C. for 15 h to obtain the final product, which was labeled as metal-organic framework material B.

Embodiment 3

[0039] Weigh 0.1g of sodium dodecylsulfonate and 0.6g of HKUST-1 seed crystals, add them into 20mL of ethanol, and ultrasonicate for 20min with a power of 300W to prepare mixed slurry A; weigh 21g of copper nitrate trihydrate, 10.08g Trimellitic acid was added to a mixed solution of 600mL of ethanol and DMF, wherein 420mL of ethanol and 180mL of DMF were prepared to obtain solution B; the mixed slurry A and solution B were mixed, and the solution was stirred at 200rpm at a temperature of 75°C for reaction and maintained After 20 hours, the reaction solution was filtered, ultrasonicated at a power of 300 W for 20 minutes during the soaking process, and the washed product was dried at 100° C. for 20 hours to obtain the final product, which was labeled as metal organic framework material C.

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Abstract

The invention discloses a metal organic framework material HKUST-1 and a preparation method thereof. The preparation method comprises: (1) adding HKUST-1 crystal seed to a first solvent, and performing first ultrasonic treatment to obtain a crystal seed-containing mixed slurry A; (2) adding trimesic acid and a copper salt to a second solvent, and dissolving to obtain a solution B; and (3) mixing the solution B and the mixed slurry A, carrying out a synthesis reaction under heating reflux and stirring, filtering after the synthesis reaction, washing, and drying to obtain the metal organic framework material HKUST-1. According to the present invention, with the method, the crystallization reaction can be accelerated, the crystal nucleus growth period of the product is shortened, the relativecrystallinity of the product can be improved, the generation of the miscellaneous crystals can be reduced, the yield of the metal organic framework material HKUST-1 can be substantially improved, andthe production cost of the product can be reduced.

Description

technical field [0001] The invention relates to a metal organic framework material HKUST-1 and a preparation method thereof. Background technique [0002] Metal-organic framework materials (Metal-Organic Frameworks, referred to as MOFs) are organic ligands containing oxygen or nitrogen elements and transition metal ions self-assembled through metal-ligand complexation network zeolite-like framework materials, with porosity High, large specific surface area, regular pore structure, easy modification and adjustable surface chemical groups, etc., have great application prospects in gas separation, adsorption, catalysis and many other aspects. [0003] At present, metal-organic framework materials are mostly synthesized by water / solvothermal synthesis. Such as Yan et al. (Xinlong Yan, Sridhar Komarneni, Zhanquan Zhang et al. Extremely enhanced CO 2 uptake by HKUST-1 metal-organic framework via a simple chemical treatment[J].Microporous and Mesoporous Materials, 2014, 183(0): ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C63/307
CPCC07C51/418C07C63/307
Inventor 邢兵张英赵亮王海洋马蕊英王刚
Owner CHINA PETROLEUM & CHEM CORP
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