Polyacid-based metal organic framework crystal material and preparation method thereof

A technology of organic frameworks and crystal materials, applied in chemical instruments and methods, catalyst activation/preparation, organic compound/hydride/coordination complex catalysts, etc., can solve the problems of poor catalytic activity and difficulty, and achieve the goal of maintaining catalytic active effect

Inactive Publication Date: 2018-02-23
HARBIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the difficulty of synthesizing polyacid-based metal-organic framework crystal materials with nanopores using the prior art and the problem of poor catalytic activity of traditional polyacids as catalysts, and to provide a flexible ligand assembly with nanopores Polyacid-based metal-organic framework crystal material and preparation method thereof

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  • Polyacid-based metal organic framework crystal material and preparation method thereof
  • Polyacid-based metal organic framework crystal material and preparation method thereof
  • Polyacid-based metal organic framework crystal material and preparation method thereof

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specific Embodiment approach 1

[0026] Embodiment 1: This embodiment is a polyacid-based metal-organic framework crystal material with nanopores assembled by flexible ligands. The chemical formula is {[Cu I (btpe) 2 ][Cu II 2 (H 2 O) 2 (btpe) 2 ][BW 12 o 40 ]}·2H 2 O, where btpe is 1,5-bistriazole-pentane; crystal system is triclinic; space group is P `1; unit cell parameters are a=89.225(5), b=74.334(5), g =70.858(5), a=12.404(5) Å, b=12.743(5) Å, c=13.447(5) Å, z=1.

[0027] {[Cu described in this embodiment mode I (btpe) 2 ][Cu II 2 (H 2 O) 2 (btpe) 2 ][BW 12 o 40 ]}·2H 2 Cu in O I The valence is +1, the coordination mode is 2 coordination, Cu II The valence is +2, and the coordination mode is 6 coordination.

[0028] Compared with the prior art, this embodiment has the following characteristics:

[0029] The present invention adopts a simple one-step hydrothermal synthesis method to successfully prepare a polyacid with nanopores assembled by flexible ligands by using 1,5-bistriazole...

specific Embodiment approach 2

[0030] Embodiment 2: This embodiment is a method for preparing a polyacid-based metal-organic framework crystal material with nanopores assembled by flexible ligands, which is completed in the following steps:

[0031] 1. Prepare a reaction solution with a pH value of 4.0: Dissolve borotungstic acid, copper acetate, and 1,5-bistriazole-pentane organic ligand into deionized water to obtain a reaction solution; adjust the pH value of the reaction solution to 4.0, to obtain a pH value of 4.0 reaction solution;

[0032] The molar ratio of borotungstic acid to metal copper salt described in step 1 is: 0.1: (0.2-1);

[0033] The molar ratio of the borotungstic acid described in step 1 to the tetrazolium-containing organic ligand is: 0.1: (0.2-0.5);

[0034] The volume ratio of the amount of borotungstic acid described in step 1 to distilled water is: 0.1mmol: (20ml-35ml);

[0035] 2. Add the reaction solution with a pH value of 4.0 into a polytetrafluoroethylene reactor, react at ...

specific Embodiment approach 3

[0039] Embodiment 3: The difference between this embodiment and Embodiment 2 is that the metal copper salt described in step 1 is copper acetate, copper nitrate or copper chloride. Others are the same as in the second embodiment.

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Abstract

The invention provides a polyacid-based metal organic framework crystal material and a preparation method thereof and relates to a polyacid-based metal organic framework crystal material with nano porous channels. The invention aims at solving the problems that the polyacid-based metal organic framework material synthesized by adopting the prior art generally has a single porous channel, the finally obtained material does not have the porous channels after a polyacid molecule is immobilized, and therefore, the catalytic activity of the material is low. A chemical formula of the designed and developed flexible ligand assembled polyacid-based metal organic framework material with the nano porous channels is {[CuI(btpe)2][CuII2(H2O)2(btpe)2][BW12]40}}.2H2O. The preparation method comprises the following steps: dissolving borotungstic acid, copper acetate and 1,5-bis(triazole)-pentane into deionized water, regulating pH value, and then carrying out reaction for 3 days at the temperature of160 DEG C. By carrying out the preparation method provided by the invention, the flexible ligand assembled polyacid-based metal organic framework crystal material with the nano porous channels can beobtained.

Description

technical field [0001] The invention relates to a flexible ligand-assembled polyacid-based metal-organic framework crystal material with nanopores. Background technique [0002] Polyoxometalates (POMs for short) is the abbreviation of polyoxometalates, which is an important part of contemporary inorganic chemistry. Compared with traditional solid acid catalysts, polyoxometalates have higher catalytic activity, and the catalytic chemical reaction conditions are generally It has become a new type of green catalyst due to its mild nature, low toxicity, and few catalytic by-products, and has received extensive attention and in-depth research. Polyacids have excellent redox properties and Brönsted acid properties, and their composition elements are adjustable. Its own oxidation-reduction potential is easy to control. At the same time, due to the "pseudo-liquid phase" reaction field of polyacid, the reaction can not only be carried out on the surface, but also inside the bulk phas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J27/188B01J35/10B01J37/08
CPCB01J27/188B01J31/34B01J35/0033B01J35/10B01J37/08
Inventor 庞海军沈清波马慧媛张春晶
Owner HARBIN UNIV OF SCI & TECH
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