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Multi-acid-based microporous crystalline material and preparation method thereof

A microporous and crystalline technology, applied in the field of polyacid-based microporous crystalline materials, can solve problems such as no pore structure

Active Publication Date: 2018-02-23
QIQIHAR UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the relatively fixed coordination mode and spatial configuration of a single ligand, the final material often does not have a pore structure, and polyacid-based microporous crystalline materials are still rarely reported.

Method used

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  • Multi-acid-based microporous crystalline material and preparation method thereof
  • Multi-acid-based microporous crystalline material and preparation method thereof
  • Multi-acid-based microporous crystalline material and preparation method thereof

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Effect test

preparation example Construction

[0030] A kind of preparation method of polyacid-based microporous crystalline material, its preparation method is as follows:

[0031] Step 1. Prepare a reaction solution with a pH value of 3 to 5: dissolve silicotungstic acid, metal cobalt salt, and 3,5-bis(4-pyridyl)pyridine into distilled water to obtain a reaction solution, and then adjust the pH of the reaction solution to Value is adjusted to 3~5, obtains the reaction liquid that pH value is 3~5;

[0032] Step 2. Preparation of a polyacid-based microporous crystalline material with a three-dimensional metal-triligand nanopore structure: add a reaction solution with a pH value of 3 to 5 into a polytetrafluoroethylene reactor, and then heat the reaction solution at a temperature of 160°C The reaction solution was lowered to room temperature for 4 days, and the reaction solution was cooled to room temperature and filtered to obtain reddish-brown blocky polyhedral crystals, which were polyacid-based micropores with a three-d...

Embodiment

[0040] Test 1. The chemical formula of a polyacid-based microporous crystalline material with a three-dimensional metal-triligand nanopore structure in this test is Co 2 (bpy)(bpp)(bip)(H 2 O) 3 [SiW 12 o 40 ], where bpy is 3,4-bipyridine, bbp is 3,5-bis(4-pyridyl)pyridine, and bip is 3,3'-bis(4-pyridyl)bipyridine; the crystal appearance is reddish-brown block shaped hexahedral crystal; the crystal system is orthorhombic; the space group is Pna2(1); the unit cell parameters are α=90°, β=90°, γ=90°, Z=4.

[0041] Test two, the method for preparing the polyacid-based microporous crystalline material with three-dimensional metal-triligand nanopore structure as described in test one is completed in the following steps:

[0042] 1. Prepare a reaction solution with a pH value of 4.0: Dissolve 0.2mmol of silicotungstic acid, 0.6mmol of metal cobalt salt, and 0.4mmol of 3,5-bis(4-pyridyl)pyridine into 18mL of distilled water to obtain the reaction liquid, then the pH value of...

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Abstract

The invention discloses a multi-acid-based microporous crystalline material and a preparation method thereof, and relates to the technical field of multi-acid-based microporous crystalline materials.The multi-acid-based microporous crystalline material has a chemical formula of Co2(bpy)(bpp)(bip)](H2O)3][SiW12O40]. The preparation method of the multi-acid-based microporous crystalline material comprises the following steps of 1, preparing reaction liquid with a pH value being 3 to 5; dissolving silicotungstic acid, metal cobalt salt and 3,5-bis(4-pyridyl)pyridine into distilled water to obtain reaction solution; then, regulating a pH value of the reaction liquid to be 3 to 5 to obtain the reaction liquid with the pH value being 3 to 5; 2, preparing the multi-acid-based microporous crystalline material with a three-dimensional metal-three-ligand nanometer pore passage structure; adding the reaction liquid with the pH value being 3 to 5 into a polytetrafluoroethylene reaction kettle; then, performing reaction at 160 DEG C for 4 days; lowering the temperature of the reaction liquid to room temperature; performing suction filtration on the reaction liquid to obtain reddish brown blocky polyhedron crystals. The multi-acid-based microporous crystalline material and the preparation method solve the problems of relatively fixed charges, coordination modes and steric configuration of single ligands of the conventional method for preparing a multi-acid-based microporous crystalline hybrid material.

Description

Technical field: [0001] The invention relates to a polyacid-based microporous crystalline material and a preparation method thereof, belonging to the technical field of polyacid-based microporous crystalline materials. Background technique: [0002] Porous metal-organic framework materials have always attracted the attention of scientists because of their excellent structure and potential applications. Therefore, how to rationally design and control the reaction process to generate porous MOFs materials is also very critical, because during the synthesis process, such as There are some difficulties in the construction process due to the influence of temperature, solvent, and pH value, as well as auxiliary ligands, so how to better design stable target porous MOFs materials is very challenging for chemists. A very important synthetic method in the field of complex chemistry, in situ metal / organic ligand reaction as a new organic reaction has become a new research method In si...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J31/34
CPCC08G83/008B01J27/188B01J31/1691B01J2531/0213B01J2531/845B01J35/39
Inventor 张转芳黄孝明徐亮陈瑶张丽赵楠
Owner QIQIHAR UNIVERSITY
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