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Copper-azole microporous crystalline material and preparation method thereof

A technology of crystal materials and pore crystals, applied in the field of porous crystalline materials and their preparation, can solve problems such as difficult to control structures, insufficient pore strength, and pore collapse, and achieve the effect of regular material structure and uniform pore size

Inactive Publication Date: 2012-07-04
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Synthesizing nanoporous coordination polymer materials is a very challenging task. It is relatively easy to design materials with a certain molecular structure, but it is difficult to control its structure in actual synthesis. The main problems are: (1) stability properties, the strength of the pores in the material is not enough, and the structure of the pores collapses when the guest molecules are removed
However, this type of immobilization is currently limited to the use of organic polymers and molecular sieves

Method used

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  • Copper-azole microporous crystalline material and preparation method thereof
  • Copper-azole microporous crystalline material and preparation method thereof
  • Copper-azole microporous crystalline material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] 0.1023g (0.6mmol) of CuCl 2 2H 2 O, 0.0449g (0.1mmol) of the ligand tris-(4-tetrazolylphenyl)amine (H 3 TCPZ) and 6mL N,N-dimethylformamide (DMF) were added to a 15mL autoclave, heated to 170°C in a closed manner and kept for 72 hours, and then cooled to room temperature at a rate not higher than 10°C / h. Filter, wash with water, and dry at room temperature to obtain 0.0404 g of bright yellow hexagonal prism crystals with a yield of 70%.

[0024] Confirmed by single crystal X-ray analysis, the product crystal prepared in the present embodiment, its structure is hexagonal crystal system, molecular formula is {[Cu(HTCPZ) 0.5 ]} ∞ , the specific parameters are listed in Table 1 below.

[0025] Table 1 Porous crystalline materials {[Cu(HTCPZ) 0.5 ]} ∞ parameter

[0026]

[0027]

[0028] figure 1 Is prepared catalyst {[Cu(HTCPZ) in the present invention 0.5 ]} ∞ A schematic diagram of the crystal structure, the crystal material is a porous material, and its p...

Embodiment 2

[0034] 0.1023g (0.6mmol) of CuCl 2 2H 2 O, 0.0449g (0.1mmol) of the ligand tris-(4-tetrazolylphenyl)amine (H 3 TCPZ) and 6mL N,N-dimethylformamide (DMF) were added to a 15mL autoclave, heated to 170°C in a closed manner and kept for 72 hours, and then cooled to room temperature at a rate not higher than 10°C / h. Filter, wash with water, and dry at room temperature to obtain 0.0346 g of bright yellow hexagonal prism crystals with a yield of 60%. Single crystal X-ray analysis confirmed that its structure is hexagonal system, molecular formula is {[Cu(HTCPZ) 0.5 ]}∞ .

[0035] The solvent used in the above examples can be selected from N,N-dimethylformamide, N,N-diethylformamide, N,N-dimethylacetamide or water.

[0036] The copper salt may be selected from copper chloride, copper bromide, copper iodide, cuprous chloride, cuprous bromide, cuprous iodide or hydrates thereof; divalent copper salts may be preferred, particularly preferably chlorinated copper.

[0037] The molar ...

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Abstract

The invention discloses a nano porous crystalline material {[Cu (HTCPZ) 0.5]} infinity and a preparation method thereof. The preparation method of the nano porous crystalline material is characterized in that: 3-(4-tetrazole-phenyl) amine and copper chloride are subjected to solvothermal synthesis according to a molar ratio of 1:(3-15) at a temperature of 80-180 DEG C; the molecular formula of the obtained Cu-based microporous crystalline material is {[Cu (HTCPZ) 0.5]} infinity, wherein HTCPZ is 3-(4-tetrazole-phenyl) amine which is a tridentate ligand having the following molecular structure shown in the accompany drawing; and the porous crystalline material is a hexagonal system crystalline material, the space group is P6122, the size range of a pore canal is 1-1.2nm, and the inner surface of the pore canal contains a coordinatively unsaturated surface of metal Cu. The preparation method provided by the invention has the advantages of simpleness, mild reaction conditions, high yield and high purity of products. The porous crystalline material prepared by the invention has the advantages of uniform pore canal, nanopore size, and metal center immobilizing.

Description

technical field [0001] The invention belongs to the field of material chemistry, and in particular relates to a porous crystalline material with copper-azole functionalized nano-sized pores and a preparation method thereof. Background technique [0002] Nanomaterials are the frontier of contemporary scientific research. When the size of ordinary materials reaches the nanometer level, it can produce surface effects, volume effects, quantum effects and macroscopic quantum tunneling effects, making nanomaterials have optical, electrical, thermal, magnetic, chemical and mechanical properties. And other aspects of the strange and excellent performance. Nanoporous materials have become a research hotspot in chemistry, physics and materials science because of their properties such as adsorption, separation, storage and catalysis brought about by their nanopores. Before the 1990s, nanoporous materials were divided into two categories: zeolite-like inorganic materials and activated ...

Claims

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Application Information

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IPC IPC(8): C07F1/08C07D257/04
Inventor 魏开举倪佳许冬至闵元增郑玉船刘扬中
Owner UNIV OF SCI & TECH OF CHINA
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