Double-metal MOF (Metal-Organic Framework) catalyst as well as preparation method and application thereof

A bimetallic and catalyst technology, applied in the field of material and chemical process research, can solve the problems of long reaction cycle, increased equipment investment cost, high reaction temperature, etc., to reduce cumbersome procedures and energy consumption, improve reaction safety performance, selectivity and The effect of high yield

Inactive Publication Date: 2018-11-09
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] (1) A large amount of catalyst is used in the reaction process, and the catalyst-product after the reaction is not easy to separate, which not only causes waste of resources, but also causes environmental pollution;
[0009] (2) A large amount of acid needs to be added in the reaction process to produce a large amount of salty wastewater, which makes the wastewater treatment process extremely complicated, which is not conducive to industrial scale-up, and puts forward higher requirements for the

Method used

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  • Double-metal MOF (Metal-Organic Framework) catalyst as well as preparation method and application thereof
  • Double-metal MOF (Metal-Organic Framework) catalyst as well as preparation method and application thereof
  • Double-metal MOF (Metal-Organic Framework) catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The preparation method of Ce-Cu-MOF-1: the molar ratio of cerium nitrate hexahydrate and copper nitrate trihydrate is 1:6, the molar ratio of the ligand tribenzoic acid to the total metal precursor is 0.2, solvent ethanol and deionized water (same volume) and the total metal precursor molar ratio is 0.1, mix the bimetallic precursor, ligand and solvent and stir at room temperature for 30min; transfer it to the reactor and react at 80°C for 12h; after the reaction, The samples were filtered, washed and dried for later use.

[0035] The Ce-Cu-MOF-1 prepared in this example is a three-dimensional cage structure with a specific surface area of ​​682 cm 2 / g, the pore volume is 0.35cm 3 / g, the average pore size is 2.03nm; its structure schematic diagram is as follows figure 1 As shown, the element Ce replaces part of the element Cu to form a bimetallic MOF material.

[0036] The XRD diffraction pattern of the bimetallic MOF material prepared in this example is shown in ...

Embodiment 2

[0039] The preparation method of Ce-Cu-MOF-2: the molar ratio of cerium nitrate hexahydrate and copper nitrate trihydrate is 6:1, the molar ratio of ligand trimesic acid to total metal precursor is 2.0, solvent ethanol and deionized water (same volume) to the total metal precursor molar ratio is 1.4, the bimetallic precursor, without stirring at room temperature, is directly transferred to the reactor and reacted at 100 ° C for 24 hours; after the reaction, the sample is filtered, washed, Dry and set aside.

[0040] The Ce-Cu-MOF-2 prepared in this example is a three-dimensional cage structure with a specific surface area of ​​176 cm 2 / g, the pore volume is 0.18cm 3 / g, the average pore diameter is 3.65nm.

[0041] The synthesized Ce-Cu-MOF-2 was used as a catalyst in the fixed-bed reaction of catalytic oxidation of p-diethylbenzene to p-ethylacetophenone. The reaction conditions are that the purity of the p-diethylbenzene raw material is 90wt%, and the volumetric space ve...

Embodiment 3

[0043] The preparation method of Ce-Cu-MOF-3: the molar ratio of cerium nitrate hexahydrate and copper nitrate trihydrate is 2:5, the molar ratio of ligand trimesic acid to total metal precursor is 0.2, solvent ethanol and deionized water (same volume) and the total metal precursor molar ratio is 0.8, mix the bimetallic precursor, ligand and solvent and stir at room temperature for 30min; transfer it to the reactor and react at 100°C for 24h; after the reaction, The samples were filtered, washed and dried for later use.

[0044] The Ce-Cu-MOF-3 prepared in this example is a three-dimensional cage structure with a specific surface area of ​​462 cm 2 / g, the pore volume is 0.27cm 3 / g, the average pore diameter is 2.86nm.

[0045] The XRD diffraction pattern of the bimetallic MOF material prepared in this example is shown in figure 2 Ce-Cu-MOF-3 in.

[0046] The synthesized Ce-Cu-MOF-3 was used as a catalyst in the fixed-bed reaction of catalytic oxidation of p-diethylbenze...

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Abstract

The invention relates to a double-metal MOF (Metal-Organic Framework) catalyst. Two inorganic metal centers and an organic ligand are self-assembled through a coordination bond to form a three-dimensional cage-shaped structure; the specific surface area is 170 to 1,145m<2>/g, the pore capacity is 0.18 to 0.48cm<3>/g and the average pore diameter is 1.34 to 3.55nm; any two types of nitrate of metalcopper, nickel, cobalt and cerium are used as metal precursors, one of trimesic acid, 2-methylimidazole or terephthalic acid is used as a synthesis ligand and a suitable solvent is selected to synthesize the double-metal MOF catalyst. A double-metal MOF material is used as a catalyst and p-diethylbenzene is used as a raw material; the p-diethylbenzene is catalytically oxidized in a fixed bed to prepare p-ethylacetophenone. The method provided by the invention has the advantages of mild reaction conditions, simplicity in operation, high p-diethylbenzene conversion rate and high p-ethylacetophenone selectivity; a product and the catalyst are easy to separate and the catalyst is stable in performance; reaction is applied to fixed bed reaction to realize continuous production, so that the method has a wide industrial application prospect.

Description

technical field [0001] The invention relates to a bimetallic MOF catalyst, a preparation method and an application, and belongs to the field of material and chemical technology research. Background technique [0002] p-Ethylacetophenone is a chemical that has attracted much attention at home and abroad in recent years. It is widely used in the production of fine chemicals such as photochromic materials, drugs, and liquid crystals, and has broad development prospects. At present, there is no large-scale production of p-ethylacetophenone in China, and the industrial use of p-ethylacetophenone mainly depends on imports. Therefore, the development of a green, simple and economical synthesis process of p-ethylacetophenone has a huge market prospect. [0003] The traditional production process of p-ethylacetophenone is the Friedel-Crafts acylation reaction, but the large amount of catalyst used in this reaction and the difficulty in recovery make this reaction difficult to apply o...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J35/10C07C45/28C08G83/00C07C49/76
CPCB01J31/1815B01J31/223B01J35/1019B01J35/1023B01J35/1028B01J35/1038B01J35/1057B01J35/1061B01J2231/70B01J2531/16B01J2531/38B01J2531/845B01J2531/847C07C45/28C08G83/008C07C49/76
Inventor 王海燕崔群许如霞顾静
Owner NANJING UNIV OF TECH
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