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Three-dimensional porous metal zinc coordination polymer and preparation method and application thereof

A coordination polymer, three-dimensional porous technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of poor product adsorption performance, complicated operation process, low yield, etc., and achieve good adsorption performance and high product purity , the effect of good thermal stability

Active Publication Date: 2019-06-28
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Choosing a rigid ligand with a larger size is conducive to the formation of a MOFs structure with high porosity. MOFs prepared by traditional hydrothermal methods will have a large amount of precipitation during the crystallization process, which needs to be cleaned with a solvent, and the post-processing operation process is complicated. The yield is low, and it is easy to form an interspersed structure with small or no pores, and the prepared product has poor adsorption performance

Method used

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  • Three-dimensional porous metal zinc coordination polymer and preparation method and application thereof
  • Three-dimensional porous metal zinc coordination polymer and preparation method and application thereof
  • Three-dimensional porous metal zinc coordination polymer and preparation method and application thereof

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[0029] A preparation method of a three-dimensional porous metal zinc coordination polymer, comprising the following steps:

[0030] 1) 1,3,5-tris(4-carboxyphenyl)benzene, N,N'-bis(4-pyridyl)-1,4,5,8-naphthalene tetracarbonyl imide and nitric acid Zinc is added to the mixed solvent of N,N-dimethylacetamide (DMA) and methanol in a molar ratio of 2:2:(2-4), and the volume ratio of DMA and water is (1-2):1 , dissolved completely after ultrasonication for 5 min.

[0031] 2) Transfer the mixed solution described in step 1) to a hydrothermal reaction kettle for solvothermal reaction, and react at 90-120° C. for 48-96 hours under autogenous pressure conditions.

[0032] 3) The reaction solution described in step 2) was lowered to room temperature at a rate of 2-5°C / h to obtain red blocky crystals, which were washed with DMA solvent, filtered, and dried naturally to obtain the three-dimensional porous metal zinc coordination polymerization thing.

[0033] Application of a three-dime...

Embodiment 1

[0036] A preparation method of a three-dimensional porous metal zinc coordination polymer, comprising the following steps:

[0037] 1) 1,3,5-tris(4-carboxyphenyl)benzene, N,N'-bis(4-pyridyl)-1,4,5,8-naphthalene tetracarbonyl imide and nitric acid Zinc is added to the mixed solvent of N,N-dimethylacetamide (DMA) and methanol at a molar ratio of 1:1:1, the volume ratio of DMA and methanol is 1:1, and it is completely dissolved after ultrasonication for 5 minutes;

[0038] 2) Transfer the mixed solution described in step 1) to a hydrothermal reaction kettle for solvothermal reaction, and react for 72 hours under autogenous pressure conditions at 90°C;

[0039] 3) The reaction solution described in step 2) was cooled to room temperature at a rate of 2° C. / h to obtain red blocky crystals, which were washed with DMA solvent, filtered, and dried naturally to obtain the three-dimensional porous metal zinc coordination polymer.

[0040] This embodiment can obtain the {[Zn that product...

Embodiment 2

[0042] A preparation method of a three-dimensional porous metal zinc coordination polymer, comprising the following steps:

[0043]1) 1,3,5-tris(4-carboxyphenyl)benzene, N,N'-bis(4-pyridyl)-1,4,5,8-naphthalene tetracarbonyl imide and nitric acid Zinc is added to the mixed solvent of N,N-dimethylacetamide (DMA) and methanol at a molar ratio of 2:2:3, the volume ratio of DMA and methanol is 2:1, and it is completely dissolved after ultrasonication for 5 minutes;

[0044] 2) Transfer the mixed solution described in step 1) to a hydrothermal reaction kettle for solvothermal reaction, and react for 48 hours under autogenous pressure conditions at 100°C;

[0045] 3) The reaction liquid described in step 2) was lowered to room temperature at a rate of 3° C. / h to obtain red blocky crystals, which were washed with DMA solvent, filtered, and dried naturally to obtain the three-dimensional porous metal zinc coordination polymer.

[0046] This embodiment can obtain the {[Zn that producti...

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Abstract

The invention discloses a three-dimensional porous metal zinc coordination polymer and a preparation method and application thereof. The chemical formula of the related polymer is {[Zn3L2(DPNDI)] 15H2O 5DMA}n, the polymer is an orthogonal crystal system, and a space group is Pban, wherein L is 1,3,5-tri(4-carboxyphenyl)benzene, and DPNDI is N,N'-di(4-pyridyl)-1,4,5,8-naphthalenetetracarboxdiimide.The complex is prepared through a solvothermal method and is of a three-dimensional porous structure, and the volume of a pore cavity is 52.0% of the total volume of single cells. The complex has good thermal stability and relatively good adsorption performance on nitrogen. Synthetic raw materials are easy to obtain, the preparation process is simple, the operation is convenient, the yield is high, and the polymer is a novel gas storage material.

Description

technical field [0001] The invention belongs to the field of preparation of functional porous coordination polymer materials, in particular to a three-dimensional porous metal zinc coordination polymer and its preparation method and application. Background technique [0002] Porous metal-organic frameworks (Metal-Organic Frameworks, MOFs) materials are a new type of porous hybrid materials that are different from traditional porous materials. Metal ions or clusters are connected by organic ligands to form an ordered three-dimensional framework with a high degree of Crystalline state, large specific surface area, easy modification and regulation, etc. It has shown rich application value in energy gas storage, selective separation, catalysis, small molecule recognition, etc., and has been an international academic research hotspot in recent years. Choosing a rigid ligand with a larger size is conducive to the formation of a MOFs structure with high porosity. MOFs prepared by ...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J20/22
Inventor 曹丽慧唐小涵刘欣徐小倩王梦马养民
Owner SHAANXI UNIV OF SCI & TECH
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