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Preparation and application of MOF-supported bimetallic catalyst

A catalyst and bimetallic technology, which is applied in the field of preparation of MOF-supported bimetallic catalysts, can solve the problems of impaired stability, need to improve stability, and reduced activity, and achieve the effects of low stability, stable activity, and difficulty in agglomeration

Active Publication Date: 2019-11-12
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the catalyst prepared by co-precipitation method has high catalytic activity, its selectivity is mostly around 50%, which needs to be improved.
In particular, the activity of the catalyst will be reduced because the bimetallic nanoparticles are easy to sinter at high temperature during use, and its stability needs to be improved.
The Chinese patent "Preparation Method of Catalyst for Hydrogenation of Carbon Dioxide to Methanol" (publication number: CN109772342A) discloses a bimetallic catalyst prepared by loading copper and zinc on the surface of mesoporous silica by co-precipitation method, However, it is inevitable that copper and zinc nanoparticles will be agglomerated during the high-temperature reaction and the stability will be impaired.

Method used

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  • Preparation and application of MOF-supported bimetallic catalyst
  • Preparation and application of MOF-supported bimetallic catalyst
  • Preparation and application of MOF-supported bimetallic catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] CuZnO x Preparation and application of @UiO-66 catalyst.

[0033] MOF (UiO-66) can be purchased commercially or synthesized by itself. The preparation method of MOF (UiO-66) in this example is as follows:

[0034] Add 0.912g of terephthalic acid, 1.280g of zirconium chloride, 320mL of N,N-dimethylformamide (DMF), and 14mL of glacial acetic acid into a hydrothermal kettle, react at a temperature of 393.25K for 24h, and take out the natural cool down. After cooling to room temperature, it was centrifuged to obtain a white solid. The product was washed more than 3 times with DMF, and after removing excess reactants, solvent replacement was performed with ethanol. The replacement followed a small number of times, 30mL to 50mL of ethanol each time, and replaced once every 24h. After more than 3 replacements, vacuum drying was performed to obtain a white solid powder MOF (UiO-66).

[0035] CuZnO x The preparation method of @UiO-66 catalyst is as follows:

[0036] 1) Wei...

Embodiment 2

[0047] First, disperse 1.0g of carrier MIL-100 in 50mL of dichloromethane, ultrasonically and stir until uniformly dispersed, and at the same time prepare 1mL of copper nitrate aqueous solution with a concentration of 0.50g / mL, and slowly add it dropwise into dichloromethane, and stir for 12h , and Cu was obtained after vacuum drying 2+ @MIL-101. Then, the Cu 2+ @MIL-101 placed in a fixed bed reactor with 5% H 2 -Ar mixed gas was reduced at 250°C to obtain Cu@MIL-101. Finally, the prepared Cu@MIL-101 was added to 50 mL of tetrahydrofuran, ultrasonically and stirred until uniformly dispersed, then 0.5 g of platinum acetylacetonate was added, stirred for 12 hours under an inert atmosphere, centrifuged, washed with THF for 3 times, vacuum Cu / PtO after drying x @MIL-101.

[0048] The Cu / PtO@MIL-101 was loaded into the fixed bed reactor, and the 2 After reduction, change the reaction gas (H 2 / CO 2 / N 2 ), adjust the temperature, gas velocity, and pressure to carry out the...

Embodiment 3

[0050] First, disperse 1.0g of carrier MIL-101 in 50mL of carbon tetrachloride, ultrasonically and stir until uniformly dispersed, and at the same time prepare 1mL of platinum chloride aqueous solution with a concentration of 0.10g / mL, and slowly add it dropwise into carbon tetrachloride , stirred for 12h, and dried under vacuum to obtain Pt 2+ @MIL-101. Then, Pt 2+ @MIL-101 placed in a fixed bed reactor with 5% H 2 -Ar mixed gas was reduced at 250°C to obtain Pt@MIL-101. Finally, the prepared Pt@MIL-101 was added to 50 mL of tetrahydrofuran, ultrasonically and stirred until uniformly dispersed, then 1.2 mL of diethylzinc in tetrahydrofuran (1 moL / L) was added under an inert atmosphere, and stirred under an inert atmosphere After 12 hours, it was separated by centrifugation, washed three times with tetrahydrofuran, and dried in vacuum to obtain Pt / ZnO@MIL-101.

[0051] Pt / ZnO x @MIL-101 is loaded into a fixed bed reactor and passed through H 2 After reduction, change the...

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Abstract

The invention discloses preparation and application of an MOF-supported bimetallic catalyst, and belongs to the technical field of catalysts. The preparation method of the catalyst comprises the following steps: 1) firstly, dispersing an MOF carrier in a hydrophobic solvent, then dropwise adding an aqueous solution of a first metal salt, carrying out ultrasonic stirring, then drying a product, andfinally reducing the dried product to reduce first metal salt ions into first metal; and 2) dispersing the product reduced in the step 1) in an organic solvent, adding a second metal organic salt inan inert atmosphere, stirring the solution, separating the obtained product, and washing and drying the product to obtain the MOF supported bimetallic catalyst. The MOF supported bimetallic catalyst is applied to CO2 hydrogenation to prepare methanol. Compared with a traditional Cu / ZnO catalyst, the catalyst has the advantages that under the same catalytic condition, the selectivity to methanol ishigher than 80%, the conversion rate is high, and the stability is greatly improved.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to the preparation and application of a MOF-supported bimetallic catalyst. Background technique [0002] Methanol is an important basic chemical and high-quality fuel. Currently, the industrial methanol production route is mainly produced from coal or natural gas through synthesis gas (carbon monoxide and hydrogen). In recent years, as the greenhouse gas carbon dioxide has attracted people's attention, the development of carbon dioxide hydrogenation to methanol technology has attracted extensive attention from academic and industrial circles. [0003] Bimetallic catalysts are the main type of catalysts currently used in the hydrogenation of carbon dioxide to produce methanol. They have high catalytic activity, low production costs and relatively simple preparation methods. Taking copper-zinc-based bimetallic catalysts as an example, the method used in the industrial production o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28B01J31/26C07C29/156C07C29/154C07C31/04
CPCB01J31/26B01J31/28C07C29/154C07C29/156C07C31/04Y02P20/52
Inventor 李军羊洋苏玉忠洪燕珍王洪涛王焱良
Owner XIAMEN UNIV
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