A kind of bimetallic organic framework nanoflower and its derivatives as well as preparation method and application

An organic framework and nanoflower technology, applied in organic compound/hydride/coordination complex catalysts, metal/metal oxide/metal hydroxide catalysts, separation methods, etc., can solve the problem of long reaction period and low reaction efficiency and other problems, to achieve a simple and gentle effect

Active Publication Date: 2022-06-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The invention solves the problems of long reaction period and low reaction efficiency of common impregnation method

Method used

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  • A kind of bimetallic organic framework nanoflower and its derivatives as well as preparation method and application
  • A kind of bimetallic organic framework nanoflower and its derivatives as well as preparation method and application
  • A kind of bimetallic organic framework nanoflower and its derivatives as well as preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Preparation of ZIF-67@CoCuBDC nanoflowers and their derivatives:

[0034] First, 0.4832g of copper nitrate trihydrate was dissolved in 14ml of DMF, and 0.3323g of terephthalic acid was dissolved in 14ml of DMF. After ultrasonication was uniform, the mixture was sonicated for 30min in an ice bath, and then placed in a water bath at 80°C for 3 days. After the reaction is completed, the obtained reaction solution A is centrifuged, washed with DMF, and then washed with methanol until the washing solution is colorless, and dried to obtain CuBDC in blue powder. Then, weigh 0.2 g of activated CuBDC, dissolve it in 10 ml of ethanol to obtain an ethanol solution of CuBDC, weigh 1.6605 g of cobalt acetate tetrahydrate, and dissolve it in 25 ml of ethanol to obtain an ethanol solution of cobalt acetate tetrahydrate; weigh 1.642 g of 2 - methylimidazole is dissolved in 25ml of ethanol to obtain the ethanolic solution of 2-methylimidazole, then the ethanolic solution of the CuBD...

Embodiment 2

[0047] (3) Different solvents in CuBDC and cobalt acetate:

[0048] First, CuBDC was prepared according to the method of Example 1. Then, 0.2 g of the activated CuBDC was weighed and dissolved in 10 ml of DMF, methanol, DMAC, and DMSO, respectively. The subsequent steps were the same as those in Example 1.

[0049] ZIF-67@CoCuBDC obtained with DMF as solvent ZIF-67@CoCuBDC obtained for H 2 The flux is 8.5*10 -7 mol·s -1 m -2 ·Pa -1 , H 2 / CO 2 and H 2 / N 2 The selectivities of 8.5 and 12.1, respectively; the obtained Co 3 O 4 / CuO can completely oxidize CO at 115℃.

[0050] ZIF-67@CoCuBDC obtained with methanol as solvent for H 2 The flux is 2.1*10 -7 mol·s -1 m -2 ·Pa -1 , H 2 / CO 2 and H 2 / N 2 The selectivities are 6.5 and 8.1, respectively; the obtained Co 3 O 4 / CuO can completely oxidize CO at 125℃.

[0051] ZIF-67@CoCuBDC obtained with DMAC as solvent for H 2 The flux is 1.6*10 -7 mol·s -1 m -2 ·Pa -1 , H 2 / CO 2 and H 2 / N 2 The selectiv...

Embodiment 3

[0054] (4) Different reaction temperatures:

[0055] First, CuBDC was prepared according to the method of Example 1. Then, weigh 0.2 g of activated CuBDC, dissolve it in 10 ml of ethanol, weigh 1.6605 g of cobalt acetate tetrahydrate, add 25 ml of ethanol; It was put into the solution of CuBDC, mixed uniformly, and then transferred to a high-pressure reactor, and reacted at 100° C., 120° C., 180° C. and 200° C. for 2 days. After the reaction is completed, wash with DMF and ethanol for 2 to 3 times respectively.

[0056] The shapes of ZIF-67@CoCuBDC obtained at different reaction temperatures are different, and the CO catalytic effect is also different.

[0057] ZIF-67@CoCuBDC for H 2 The flux is 4.5*10 -8 mol·s -1 m -2 ·Pa -1 , H 2 / CO 2 and H 2 / N 2 The selectivities of 10.8 and 12.6, respectively; the obtained Co 3 O 4 / CuO can completely oxidize CO at 125℃.

[0058] Among them, the ZIF-67@CoCuBDC obtained at 120 °C has a 2 The flux is 3.6*10 -7 mol·s -1 m ...

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Abstract

The invention discloses a double metal organic framework nano flower and its derivatives as well as a preparation method and application. The preparation method of the double metal organic framework nanoflowers is as follows: the N,N-dimethylformamide solution of the copper nitrate trihydrate and the N,N-dimethylformamide solution of the terephthalic acid are mixed in an ice bath. Dimethylformamide solution is mixed with ultrasound, reacted completely in a water bath at 50-100°C to obtain CuBDC; dissolving cobalt acetate tetrahydrate in an organic solvent to obtain a mixed solution, and after ultrasonically stirring with the ethanol solution of CuBDC, Add the ethanol solution of 2-methylimidazole, transfer it to the reaction kettle after ultrasonication, and react at 100-200°C for 2-3 days. After the reaction is complete, the obtained reaction solution B is filtered, washed, and dried to obtain the product ZIF-67 @CoCuBDC nanoflowers. The ZIF‑67@CoCuBDC was placed in an air atmosphere and calcined at 250–500 °C for 2–4 h to obtain the ZIF‑67@CoCuBDC derivative Co 3 o 4 @CoCuO nanoflowers, applied to H 2 / CO 2 or H 2 / N 2 gas separation. The ZIF‑67@CoCuBDC nanoflowers were calcined to obtain Co 3 o 4 @CoCuO nanoflowers, applied to the purification of CO.

Description

(1) Technical field [0001] The invention relates to a bimetallic organic frame nanoflower and a derivative thereof, a preparation method and application thereof. (2) Background technology [0002] Metal-organic frameworks (MOFs) are a class of organic-inorganic hybrid materials containing inorganic metal nodes and organic ligands. Compared with traditional inorganic materials, MOFs have ultra-high specific surface area; tunable pore size and shape; and easy-to-modify structure. These excellent properties make them widely used in catalysis, separation, sensing and other fields. In recent years, metal-organic frameworks with a single structure prepared by conventional methods have been unable to effectively meet some practical needs. In order to make up for this deficiency, more researchers began to modify metal-organic frameworks before and after the synthesis process. MOFs materials with more complex structures and better effects are obtained. [0003] Initially, Yaghi et ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/75B01J31/22B01J35/02B01J37/08B01J37/30B01D53/86B01D53/62B01D53/46C01B32/50
CPCB01J31/1691B01J31/1815B01J23/75B01J35/026B01J37/30B01J37/086B01J37/088B01D53/864B01D53/8671C01B32/50B01J2531/845B01D2256/10B01D2256/22Y02P20/151
Inventor 张国亮毛静雯
Owner ZHEJIANG UNIV OF TECH
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