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Preparation method of sec-butyl alcohol dehydrogenation MOF catalyst

A technology of MOF and catalyst, which is applied in the field of preparation of sec-butanol dehydrogenation MOF catalyst, can solve the problems of not being able to be used as a dehydrogenation catalyst, achieve high activity stability and product selectivity, improve conversion rate, and prevent growth

Active Publication Date: 2021-06-04
烟台市友利化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, most MOF compounds are complexes formed by a single metal ion and a ligand, which is different from the coexistence of multiple components in the actual catalyst, and cannot be used as a dehydrogenation catalyst.

Method used

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  • Preparation method of sec-butyl alcohol dehydrogenation MOF catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Method for preparing sec-butanol dehydrogenation MOF catalyst, its steps: weigh Cu (NO 3 ) 2 · 3h 2 O 25G and Zn (NO 3 ) 2 · 6h 2 O 15g is miscible in 200 ml of dimethylformamide and heated to 80 ° C, weigh Al (NO 3 ) 3 · 9h 2 O 3 g is dissolved in 100 ml of dimethylformamide and heated to 80 ° C, and 65 g of terephthalic acid was sungined in dimethylformamide dissolved in 500 ml of 80 ° C, and the Al salt solution was slowly added to benzene under vigorous stirring. In the dimethic acid solution, it was continued after completion of 2 h; in the above solution, the Cu-Zn mixed salt solution was added to the above solution, and then stirred after 2 h after addition, the above materials were transferred into the autoclave at 150 ° C for 20 h, resulting in a blue Substance, filtration, solid material drying at 120 ° C for 10 h, placed in a tubular furnace 5% o 5% o 2 / 95% N 2 Carbonization treatment for 5 h, get a black material, add 1G K 2 CO 3 The mix is ​​uniform, which is...

Embodiment 2

[0018] Method for preparing sec-butanol dehydrogenation MOF catalyst, its steps: weigh Cu (NO 3 ) 2 · 3h 2 O 60G and Zn (NO 3 ) 2 · 6h 2 O 15g is miscible in 500 ml of anhydrous ethanol and heated to 70 ° C, weigh Al (NO 3 ) 3 · 9h 2 O 10 g is dissolved in 100 ml of anhydrous ethanol and heated to 70 ° C, weighing 139 g of tamaic acid dissolved in anhydrous ethanol dissolved in 700 ml of 70 ° C, and the Al salt solution slowly added a wafer solution at a variety of stirring. In the ethanol solution, it was continued for 1 h after addition, and the Cu-Zn mixed salt solution was added to the above solution, and then stirred after 2 h after addition, the above materials were transferred into the autoclave at 250 ° C for 10 h, resulting in a blue substance , Filtration, solid material is dried in vacuo at 110 ° C for 15 h, and placed in a tubular furnace at 500 ° C for 5% o. 2 / 95% N 2 Carbonization treatment for 3 h, get a black substance, add 1.5G NA 2 CO 3 The mix is ​​uniform, wh...

Embodiment 3

[0020] Method for preparing sec-butanol dehydrogenation MOF catalyst, its steps: weigh Cu (NO 3 ) 2 · 3h 2 O 27G and Zn (NO 3 ) 2 · 6h 2 O 20G is miscible in 500 ml of dimethylformamide and heated to 80 ° C, AlCl 3 10 g is dissolved in 200 ml of dimethylformamide and heated to 80 ° C, and 85 g of terephthalic acid is soluble in dimethylformamide dissolved in 500 ml of 80 ° C, and the Al salt solution slowly adds the Al salt solution to benzene. In the formic acid solution, it was followed after 1 h after addition, and the Cu-Zn mixed salt solution was added to the above solution. After the addition is completed, stirring for 2 h, and the material was transferred into the autoclave at 200 ° C for 20 h, resulting in a blue material , Filtration, solid material drying at 120 ° C for 10 h, placed in a tubular furnace 5% by 450 ° C 2 / 95% N 2 Carbonization treatment for 5 h, get a black substance, add 1.5g K 2 CO 3 The mix is ​​uniform, which is obtained.

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Abstract

The invention discloses a sec-butyl alcohol dehydrogenation MOF catalyst preparation method, which comprises: 1) adding an Al salt to a ligand solution, heating, generating an Al pre-coordination compound, maintaining heating, adding a Cu salt and a Zn salt at the same time, and carrying out a continuous reaction to generate an Al-Cu-Zn multi-element MOF; (2) carrying out carbonization treatment on the Al-Cu-Zn multi-element MOF obtained in the step (1) under the condition of low-oxygen atmosphere, so as to prepare a skeleton carbon support body; and 3) uniformly mixing the skeleton carbon support body obtained in the step 2) with an alkali metal salt catalytic modifier. In the invention, the solvothermal method is adopted to synthesize the Cu, Zn and Al multi-element symbiotic organic coordination compound with a metal organic framework structure, metal ions are distributed at different node positions by a method of adding metal salt step by step, MOF can be generated very gently by modulating solvothermal conditions, and controllable distribution of the metal ions is ensured; and the obtained catalyst has high activity stability and product selectivity.

Description

Technical field [0001] The present invention relates to the field of organic synthesis, and more particularly to a method for preparing a sec-butanol dehydrogenation MOF catalyst. Background technique [0002] Methyl ethyl ketone is a very important chemical raw material and organic solvent, which is very wide. The main method of producing methyl ethyl ketone is to prepare Methyl ethyl ketone in secondary alcohol, which uses CuO, ZnO, Al. 2 O 3 catalyst. For example, the public will be disclosed in China's invention patents in CN100360228C and CN1101262C, respectively, Cuo, ZnO, Al 2 O 3 The methyl ethyl ketone catalyst is prepared by secondary alcohol. China Patent CN105709752A first formulates the zinc salt of an ethylenediamine complex, a mixed aqueous solution of copper salts and rare earth salts, and coprecipitation at a certain pH to obtain Cuo, ZnO, Al, ZnO, Al 2 O 3 catalyst. China Patent CN107597125B discloses Cuo, ZnO, Al containing solid potassium 2 O 3 The catalyst is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J35/10C07C49/10C07C45/29
CPCB01J31/1691B01J31/223C07C45/29B01J2531/16B01J2531/31B01J2531/26B01J35/61C07C49/10
Inventor 张慧敏
Owner 烟台市友利化工科技有限公司