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Synthetic method of polynitrogen azole zinc/cadmium framework material

A frame material, polyazole zinc technology, applied in the direction of zinc organic compounds, cadmium organic compounds, etc., can solve the problems of high cost, difficulty in activation, low reaction yield, etc., and achieve rapid reaction, accelerated reaction speed, and post-processing of products simple effect

Inactive Publication Date: 2010-09-15
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for synthesizing polyazole zinc / cadmium framework materials according to the problems of high cost, low reaction yield and difficulty in activation in the synthesis process of existing polyazole zinc / cadmium framework materials

Method used

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  • Synthetic method of polynitrogen azole zinc/cadmium framework material
  • Synthetic method of polynitrogen azole zinc/cadmium framework material
  • Synthetic method of polynitrogen azole zinc/cadmium framework material

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Embodiment 1

[0035] The room temperature efficient preparation of a small amount of MAF-4 of embodiment 1

[0036] In a 10mL ground-mouth round bottom flask, add 99.4mg Zn(OH) 2 Or 81.4mg ZnO (1.0mmol), 164.2mg Hmim (2.0mmol), 5.0mL reaction solution, capped, stirred at room temperature for 24h and then filtered. The filter cake was washed three times with methanol and dried at 120°C to obtain the product with a yield of about 95%. The reaction solution consisted of 4.0 mL of methanol and 1.0 mL of 25 wt% ammonia water during the initial synthesis. The filtrate obtained after each synthesis can be directly used as the reaction solution for the next synthesis, and can be recycled at least 5 times without reducing the purity and yield of the product.

Embodiment 2

[0037] Efficient preparation at room temperature of a large amount of MAF-4 of embodiment 2

[0038] In a 1000mL ground-mouth round bottom flask, add 99.4g Zn(OH) 2 Or 81.4g ZnO (1.0mol), 164.2g Hmim (2.0mol), 500mL reaction solution, cover, stir vigorously at room temperature for 24h, and then filter. The filter cake was washed three times with methanol and dried at 120°C to obtain the product with a yield of about 95%. The reaction solution consisted of 400mL of methanol and 100mL of 25wt% ammonia water during initial synthesis. The filtrate obtained after each synthesis can be directly used as the reaction solution for the next synthesis, and can be recycled at least 5 times without reducing the purity and yield of the product.

Embodiment 3

[0039] The microwave heating fast preparation of embodiment 3MAF-4

[0040] Add 99.4mg Zn(OH) to a 60mL microwave reactor with Teflon substrate 2 Or 81.4mg ZnO (1.0mmol), 164.2mg Hmim (2.0mmol), 5.0mL reaction solution, stirred at room temperature for a few minutes, sealed, microwave heated to 40°C for 1.5h, cooled to room temperature and filtered. The filter cake was washed three times with methanol and dried at 120°C to obtain the product with a yield of about 95%. The reaction solution consisted of 4.0 mL of methanol and 1.0 mL of 25 wt% ammonia water during the initial synthesis. The filtrate obtained after each synthesis can be directly used as the reaction solution for the next synthesis, and can be recycled at least 5 times without reducing the purity and yield of the product.

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Abstract

The invention relates to a synthetic method of a polynitrogen azole zinc / cadmium framework material. The method comprises the following steps of: mixing a polynitrogen azole ligand with a metering ratio of a metal polynitrogen azole framework chemical formula, an oxide or a hydroxide with a reaction liquid, carrying out an acid-base reaction after activation, and filtering, washing and drying after the reaction to obtain the polynitrogen azole zinc / cadmium framework material. The synthetic method has mild reaction conditions, and the polymerization process of the polynitrogen azole ligand and the solid oxide or the hydroxide is accelerated by utilizing the coordination buffer action of ammonia to enable the reaction to be rapidly and efficiently finished. The method has simple operation and low production cost and does not generate any other byproducts except a required product and water, the obtained product is easy to activate, and a residual mother liquid can be directly used as the reaction liquid for the next batch of synthesis, thereby realizing continuous production and being particularly suitable for large-scale industrialized production.

Description

technical field [0001] The invention relates to the field of preparation of porous coordination polymers, in particular to a synthesis method of polyazole zinc / cadmium frame material. Background technique [0002] Porous coordination polymers are a new type of porous materials with advantages such as low density, large specific surface area, strong chemical modifiability, and structural flexibility, and can be widely used in the fields of gas storage, separation, and heterogeneous catalysis (US 5862796; US 7196210; US 6930193; US 7196210; US 6624318; US20080121105). [0003] Compared with porous materials such as conventional inorganic zeolites, molecular sieves and activated carbon, porous coordination polymers are more sensitive to the reaction conditions of synthesis, and slight differences in reaction mechanism and conditions will lead to huge differences in the structure, yield and performance of the obtained products. Therefore, the efficient synthesis of porous coord...

Claims

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Application Information

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IPC IPC(8): C07F3/06C07F3/08
Inventor 张杰鹏朱爱新林锐标洪惠玲陈小明
Owner SUN YAT SEN UNIV
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