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Preparation and application methods of solid acid catalyst based on Zr-MOF

A solid acid catalyst and catalyst technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of strong corrosion and oxidation, low reaction yield, poor acid resistance, etc., to achieve Good economic and social benefits, good reaction stability and good reaction performance

Inactive Publication Date: 2018-09-07
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a strong mineral acid, concentrated sulfuric acid is cheap and easy to obtain, and has high activity. However, as we all know, concentrated sulfuric acid catalysis also has disadvantages that cannot be ignored: strong corrosion and oxidation, which makes it difficult to control its reaction conditions and severely corrodes production. Equipment, low reaction yield, difficult waste acid treatment, etc.
General MOF has the problems of low thermal stability and poor acid resistance, but by using some transition metals, the thermal stability and acid resistance of the material can be significantly improved
Acidified zirconia has strong acidity and can be used for reactions that require strong acid catalysis, but the specific surface area of ​​zirconia is small and the pore size distribution is uneven, so it is not conducive to shape-selective catalysis. Environmentally friendly solid acid catalyst to replace concentrated sulfuric acid catalyst has important theoretical significance and great application value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 50ml of N,N-dimethylformamide to a mixture of 0.3500g of zirconium tetrachloride and 0.2490g of 1,4-terephthalic acid, stir magnetically for 30min, ultrasonically for 10min until completely dissolved, put it into a 100ml kettle Solvothermal reaction at 120°C for 60h, suction filtration, and drying of the precipitate at 80°C for 24h to obtain white precursor powder Zr-MOF. The above-mentioned white precursor powder was calcined at 300° C. for 4 hours in an air atmosphere to obtain a white or gray porous solid. The loose porous solid obtained above was impregnated with 6mol / L toluene sulfate solution at 25°C for 24h, filtered with suction, the precipitate was washed with absolute ethanol three times and then filtered, the product was vacuum-dried at 60°C for 8h, and calcined at 350°C for 4h. A solid acid catalyst for Zr-MOF is available.

[0023] Add 15g o-xylene and 0.051g Zr-MOF solid acid catalyst to a 100mL four-neck flask equipped with a stirrer, condenser, ther...

Embodiment 2

[0026] Add 50ml of N,N-dimethylformamide to the mixture of 0.3500g of zirconium tetrachloride and 0.3630g of 4,4'-biphenyl dicarboxylic acid, stir magnetically for 30min, ultrasonic for 10min until completely dissolved, and put it into a 100ml kettle Solvothermal reaction at 120°C for 60h, suction filtration, and drying of the precipitate at 80°C for 24h to obtain white precursor powder Zr-MOF. The above-mentioned white precursor powder was calcined at 300° C. for 4 hours in an air atmosphere to obtain a white or gray porous solid. The loose porous solid obtained above was impregnated with 6mol / L toluene sulfate solution at 25°C for 24h, suction filtered, the precipitate was washed 5 times with absolute ethanol and then filtered, the product was vacuum dried at 60°C for 8h, and calcined at 350°C for 4h. A solid acid catalyst for Zr-MOF is available.

[0027] Add 15g o-xylene and 0.051g Zr-MOF solid acid catalyst to a 100mL four-neck flask equipped with a stirrer, condenser, t...

Embodiment 3

[0030]Add 50ml of N,N-dimethylformamide to a mixture of 0.3500g of zirconium tetrachloride and 0.2992g of 1,4-terephthalic acid, stir magnetically for 30min, ultrasonicate for 10min until completely dissolved, put it into a 100ml kettle Solvothermal reaction at 120°C for 60h, suction filtration, and drying of the precipitate at 80°C for 24h to obtain white precursor powder Zr-MOF. The above-mentioned white precursor powder was calcined at 300° C. for 4 hours in an air atmosphere to obtain a white or gray porous solid. The loose porous solid obtained above was impregnated with 6mol / L toluene sulfate solution at 25°C for 24h, suction filtered, the precipitate was washed 5 times with absolute ethanol and then filtered, the product was vacuum dried at 60°C for 8h, and calcined at 350°C for 4h. A solid acid catalyst for Zr-MOF is available.

[0031] Add 15g o-xylene and 0.051g Zr-MOF solid acid catalyst to a 100mL four-neck flask equipped with a stirrer, condenser, thermometer and...

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PUM

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Abstract

The invention discloses preparation and application methods of a solid acid catalyst based on Zr-MOF. The preparation method of the catalyst comprises the following steps: with zirconium tetrachlorideor zirconium oxychloride selected as a zirconium source, 1,4-terephthalic acid or biphenyl-4,4'-dicarboxylic acid as an organic ligand and DMF (N,N-dimethylformamide) as a solvent, a MOF (metal organic framework) material with network topology is synthesized with a solvothermal method, the solid acid catalyst based on zirconia is obtained by calcination in air atmosphere and acidification by strong acid. The catalyst has higher alkylation conversion rate, PXE (1-phenyl-1-xylylethane) yield and reusability at high temperature and under normal pressure.

Description

Technical field: [0001] The invention relates to the preparation and application method of a Zr-MOF-based solid acid catalyst, belonging to the technical field of industrial catalysis. Background technique: [0002] Diarylethane (1-phenyl-1-xylylethane), referred to as PXE, is a product developed by Japan and the United States in the 1970s that can replace chlorinated biphenyl-type power capacitor impregnants. . 1-phenyl-1-xylylethane (1-pHenyl-1-xylylethane, referred to as PXE) synthesized from styrene and xylene has the characteristics of high boiling point, low viscosity and low freezing point, and is widely used in Solvent for pressure-sensitive dyes of carbonless copy paper. In addition, it can also be used as organic heat carrier, plasticizer and lubricating oil for plastic processing. This reaction is often catalyzed by concentrated sulfuric acid. As a strong mineral acid, concentrated sulfuric acid is cheap and easy to obtain, and has high activity. However, as we...

Claims

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Application Information

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IPC IPC(8): B01J27/053B01J27/18B01J31/02B01J35/10B01J37/08B01J37/02C07C2/72C07C15/16
CPCC07C2/72B01J27/053B01J27/16B01J31/0225B01J37/0201B01J37/086B01J35/60C07C15/16
Inventor 盛晓莉王贝贝周钰明张一卫
Owner SOUTHEAST UNIV
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