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MOF supported metal peroxide catalyst

A metal peroxide, metal peroxide technology, applied in physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, refining with oxygen-containing compounds, etc., can solve the problem of catalyst deactivation, active group The problem of separation loss, etc., to achieve the effect of high activity, good stability, and stable catalyst activity

Inactive Publication Date: 2016-02-03
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Supported Mo-based catalysts are the most common catalysts in liquid-phase oxidation systems, and the loading methods adopted are generally impregnation or co-precipitation methods. Causes the loss of active components and leads to catalyst deactivation

Method used

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  • MOF supported metal peroxide catalyst
  • MOF supported metal peroxide catalyst
  • MOF supported metal peroxide catalyst

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Experimental program
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Effect test

preparation example Construction

[0043] About the preparation method of above-mentioned catalyst, more specific embodiment is as follows:

[0044] In MO(O 2 ) 2 , (M=Mo 6+ , W 6+ ) instead of the commonly used MO 3 (M=Mo 6+ , W 6+ ) as the main active component of the catalyst. The specific preparation steps are: weigh 2-50g MoO 3 And 15ml~500ml30% H 2 o 2Transfer the aqueous solution into a 50-1000ml round-bottom flask, stir overnight at room temperature to 90°C, filter and separate, add a certain amount of DMF solvent to the collected filtrate, refrigerate and crystallize in the refrigerator for 1-14 days, and then carry out vacuum filtration until dry. Get MoO(O 2 ) 2 2DMF. The content of the active components of the catalyst is between 5% and 50% in terms of mass fraction (calculated on the basis of the total mass of the catalyst).

[0045] Select an organic ligand containing a bipyridyl chelate coordination site to coordinate with a zirconium salt to prepare a zirconium-based metal-organic f...

Embodiment 1

[0053] Embodiment 1, the preparation of metal organic framework material

[0054] Preparation of MOF(Zr): Weigh 0.13g 2,2’-bipyridine-5,5’-dicarboxylic acid, 0.38g biphenyl dicarboxylic acid, 0.49g ZrCl 4 , dissolved in 100ml of N,N'-dimethylformamide (DMF), followed by the addition of 3.6ml of acetic acid. Reactions were carried out in 150ml round bottom flasks. After stirring at room temperature for 30 minutes, the temperature was raised to 120° C., and stirred at constant temperature for 36 hours. After suction filtration and drying, the solid was transferred to the above-mentioned round-bottomed flask, and 100 ml of DMF was added and stirred at a constant temperature in an oil bath at 80° C. for 3 h. After suction filtration and drying, the resulting solid was transferred to a Soxhlet extractor and extracted with ethanol overnight. The solid powder obtained after drying is MOF(Zr).

Embodiment 2

[0055] Embodiment 2, the preparation of metal peroxide

[0056] MoO(O 2 ) 2 Preparation: weigh 10gMoO 3 and 50ml30% H 2 o 2 The aqueous solution was transferred into a 100ml round bottom flask, stirred overnight at 45°C, filtered and separated, a certain amount of DMF solvent was added to the collected filtrate, refrigerated and crystallized in the refrigerator for three days, and then vacuum filtered to dryness to obtain MoO(O 2 ) 2 • 2DMF (8.9 g, 0.0276 mol).

[0057] WO(O 2 ) 2 Preparation of hydrogen peroxide solution: weigh tungstic acid (9.3g), measure H 2 o 2 (80ml) in the round-bottomed flask of 100ml, stirred overnight at room temperature, centrifuged then, the liquid product of collecting is WO(O 2 ) 2 of hydrogen peroxide solution.

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Abstract

The invention provides an MOF supported metal peroxide catalyst. The catalyst comprises a metal organic skeleton carrier and a metal peroxide species MO(O2)2, wherein M represents Mo6 or W6+. The catalyst is prepared in the mode that in the metal organic skeleton material synthesizing process, MO(O2)2 with catalytic oxidation activity is anchored to a metal organic skeleton material through a pre-modification or post-modification method. According to the catalyst, metal peroxide is highly dispersed on a crystal skeleton, and the metal peroxide species is coordinated with organic ligand based on dipyridyl chelation locus, so that high stability is kept; when applied to an oxidation sweetening reaction, high activity and stability are kept, and the catalyst has important industrial application value.

Description

technical field [0001] The invention belongs to the technical fields of catalysis, petroleum processing and petrochemical industry, and in particular relates to a metal organic framework immobilized metal peroxide catalyst for catalytic oxidation desulfurization and a preparation method thereof. Background technique [0002] The reality of my country's environmental pollution control needs to improve the quality of fuel. At present, hydrodesulfurization (HDS) technology is usually used in industry to remove sulfur compounds in diesel fraction. Traditional hydrodesulfurization technology can reduce the sulfur content in the diesel fraction to 300-500ppmw, and the remaining sulfur compounds are mainly fused-ring sulfur compounds such as dibenzothiophene (DBT) with low HDS activity. The hydrodesulfurization method requires very harsh reaction conditions and consumes more hydrogen to remove, resulting in a significant increase in energy consumption and operating costs. The hyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C10G27/12
Inventor 刘颖雅王安杰李翔王春花孙志超王伟
Owner DALIAN UNIV OF TECH
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