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A kind of preparation method of sec-butanol 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 that it cannot be used as a dehydrogenation catalyst, achieve high activity stability and product selectivity, improve conversion rate, and improve selectivity.

Active Publication Date: 2022-05-24
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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  • A kind of preparation method of sec-butanol dehydrogenation MOF catalyst

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Experimental program
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Effect test

Embodiment 1

[0016] Preparation method of sec-butanol dehydrogenation MOF catalyst, the step of which is: call Cu (NO 3 ) 2 ·3H 2 O25g and Zn(NO 3 ) 2 ·6H 2 O 15g miscible in 200ml of dimethylformamide and heated to 80 °C, called Al (NO 3 ) 3 ·9H 2O 3g dissolved in 100mL dimethylformamide and heated to 80 ° C, weigh terephthalic acid 65g dissolved in 500ml 80 ° C dimethylformamide, under vigorous stirring the Al salt solution slowly added to the terephthalic acid solution, after addition continue to stir for 2h; the Cu-Zn mixed salt solution was added to the above solution, after addition continue to stir for 2h, the above material was moved into an autoclave at 150 ° C reaction for 20h, to obtain a blue substance, filter, The solid material is dried in vacuum at 120 °C for 10 h and placed in a tube furnace at 450 °C with 5% O 2 / 95％N 2 Carbonized for 5h to give a black substance, 1 g K added 2 CO 3 Mix well and get.

Embodiment 2

[0018] Preparation method of sec-butanol dehydrogenation MOF catalyst, the step of which is: call Cu (NO 3 ) 2 ·3H 2 O60g and Zn(NO 3 ) 2 ·6H 2 O 15g miscible in 500 mL absolute ethanol and heated to 70 °C, called Al (NO 3 ) 3 ·9H 2 O 10g dissolved in 100mL absolute ethanol and heated to 70 °C, weighed 139g of homobenzotricarboxylic acid dissolved in 700ml of 70 °C absolute ethanol, under vigorous stirring the Al salt solution slowly added to the homohydral tricarboxylic acid anhydrous ethanol solution, continue to stir for 1h after addition; add Cu-Zn salt mixture solution to the above solution, continue to stir for 2h after addition, move the above material into an autoclave at 250 °C reaction for 10h, to obtain a blue substance, filter, The solid material is dried in a vacuum at 110 °C for 15 h and placed in a tubular furnace at 500 °C with 5% O 2 / 95％N 2 Carbonized for 3h to obtain a black substance, 1.5g Na was added 2 CO 3 Mix well and get.

Embodiment 3

[0020] Preparation method of sec-butanol dehydrogenation MOF catalyst, the step of which is: call Cu (NO 3 ) 2 ·3H 2 O27g and Zn(NO 3 ) 2 ·6H 2O20g miscible in 500 ml of dimethylformamide and heated to 80 °C, AlCl 3 10g dissolved in 200mL dimethylformamide and heated to 80 °C, weigh terephthalic acid 85g dissolved in 500ml 80 °C dimethylformamide, under vigorous stirring the Al salt solution slowly added to the terephthalic acid solution, continue to stir for 1h after addition; the Cu-Zn salt mixed solution was added to the above solution, continue to stir for 2h after addition, move the above material into an autoclave at 200 °C reaction for 20h, to obtain a blue substance, filter, The solid material is dried in vacuum at 120 °C for 10 h and placed in a tube furnace at 450 °C with 5% O 2 / 95％N 2 Carbonized for 5h to give a black substance, 1.5g K was added 2 CO 3 Mix well and get.

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Abstract

The invention discloses a preparation method of a sec-butanol dehydrogenation MOF catalyst, which comprises the following steps: 1) adding Al salt to a ligand solution first, heating to generate a pre-coordination compound of Al, keeping heating, and simultaneously Adding Cu salt and Zn salt, continuing the reaction to generate Al-Cu-Zn multi-element MOF; 2) carbonizing the Al-Cu-Zn multi-element MOF obtained in step 1) under a low-oxygen atmosphere to obtain a skeleton carbon Support body; 3) uniformly mix the skeleton carbon support body obtained in step 2) with the alkali metal salt catalytic modifier to obtain the product. The present invention adopts solvothermal method to synthesize Cu, Zn, Al multi-element symbiotic organic coordination compound with metal-organic framework structure, and distributes metal ions in different node positions by adding metal salt step by step to adjust solvothermal conditions The MOF can be formed very gently, which ensures the controllable distribution of metal ions, 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, in particular to a method for preparing a sec-butanol dehydrogenation MOF catalyst. Background [0002] Methyl ethyl ketone is a very important chemical raw material and organic solvent, and it is very versatile. At present, the main method of production of methyl ethyl ketone is the preparation of methyl ethyl ketone by sec-butanol dehydrogenation, and CuO, ZnO and Al are used in this method 2 O 3 Catalyst. For example, CuO, ZnO, and Al are disclosed in Chinese invention patents with publication numbers CN100360228C and CN1101262C, respectively 2 O 3 Catalyst for the preparation of methyl ethyl ketone from the dehydrogenation of sec-butanol. Chinese patent CN105709752A first prepared a zinc salt ethylenediamine complex, prepared a mixed aqueous solution of copper salt and rare earth salt, and co-precipitated at a certain pH to obtain CuO, ZnO and Al containing rare earth elements 2 O 3 Cataly...

Claims

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Application Information

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Patent Type & Authority Patents(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