Heteropolyacid-modified Zr-MOF catalyst as well as preparation method and application thereof

A technology of heteropolyacid and catalyst, which is applied in the field of heteropolyacid modified Zr-MOF catalyst and its preparation, which can solve the problems of poor catalytic effect and achieve strong action, high selectivity, thermal stability and chemical stability good sex effect

Inactive Publication Date: 2015-08-26
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is to provide a heteropolyacid m

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Synthesis of Zr-MOF carrier: add 0.01mol zirconium tetrachloride, 0.01mol terephthalic acid, 0.005mol cetyltrimethylammonium bromide, 0.003mol citric acid to 50mL of N,N-dimethyl In formamide (DMF), stir; after stirring until all the solids are dissolved, transfer the mixed solution to a hydrothermal synthesis kettle lined with polytetrafluoroethylene and place it in a homogeneous reactor at 220°C for 24 hours. Then cool to room temperature; filter the mixture in the reactor, and wash the filtered solid with N,N-dimethylformamide (DMF) 5 times, using 10 mL each time, and then place the solid in a vacuum at 60°C Drying in a drying box for 12 hours; the vacuum-dried solid is placed in a muffle furnace at a temperature of 300° C. and roasted for 3 hours to obtain a Zr-MOF carrier.

[0029] Synthesis of heteropoly acid / Zr-MOF: first dissolve 0.1 g of phosphotungstic acid in 15 mL of deionized water, stir to form a solution, immerse 4.9 g of the Zr-MOF carrier prepared above in...

Embodiment 2

[0032] Synthesis of Zr-MOF carrier: add 0.01mol zirconium oxychloride, 0.02mol terephthalic acid, 0.006mol cetyltrimethylammonium bromide, 0.008mol citric acid to 50mL of N,N-dimethyl Stir in formamide (DMF); after stirring until all the solids are dissolved, transfer the mixed solution to a hydrothermal synthesis kettle lined with polytetrafluoroethylene and place it in a homogeneous reactor at 220°C for 24 hours. Then cool to room temperature; filter the mixture in the reaction kettle, and wash the filtered solid with N,N-dimethylformamide (DMF) 5 times, using 10 mL each time, and then place the solid in a vacuum at 70°C Drying in a drying oven for 12 hours; the vacuum-dried solid is placed in a muffle furnace at 350° C. and roasted for 3 hours to obtain a Zr-MOF carrier.

[0033] Synthesis of heteropoly acid / Zr-MOF: first dissolve 0.1 g of phosphotungstic acid in 8 mL of deionized water, stir to form a solution, immerse 1.15 g of the Zr-MOF carrier prepared above in the phosph...

Embodiment 3

[0036] Synthesis of Zr-MOF carrier: add 0.01mol zirconium tetrachloride, 0.03mol trimesic acid, 0.001mol sodium dodecylbenzene sulfonate, 0.007mol tartaric acid to 50mL absolute ethanol, stir; stir until solid After all is dissolved, transfer the mixed solution to a hydrothermal synthesis kettle lined with polytetrafluoroethylene material, and place it in a homogeneous reactor at 250°C for 36 hours, and then cool to room temperature; change the mixed solution in the reaction kettle Filter and wash the filtered solid with absolute ethanol 5 times, using 10 mL each time, then place the solid in a vacuum drying oven at 70°C for 12 hours; place the vacuum-dried solid in a muffle furnace at 400°C to roast After 3h, Zr-MOF vector was prepared.

[0037] Synthesis of heteropoly acid / Zr-MOF: first dissolve 0.1g silicotungstic acid in 6mL deionized water, stir to form a solution, immerse 0.9g of the Zr-MOF carrier prepared above in the silicotungstic acid aqueous solution, and put it in 11...

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Abstract

The invention discloses a heteropolyacid-modified Zr-MOF catalyst which is modified by heteropolyacid through a Zr-MOF carrier. The invention further discloses a preparation method for the catalyst and an application of the catalyst to reaction of preparing acraldehyde by catalyzing glycerol dehydration. Compared with the prior art, the obtained catalyst is long in service life, and the glycerol conversation rate and the acraldehyde selectivity are high; the Zr-MOF carrier is good in thermal stability and chemical stability, and the framework structure is kept stable; theacting force between the heteropolyacid and the Zr-MOF carrier is relatively strong, so that the heteropolyacid-modified Zr-MOF catalyst is not liable to lose.

Description

Technical field [0001] The invention belongs to the field of chemical synthesis, and specifically relates to a heteropolyacid modified Zr-MOF catalyst and a preparation method and application thereof. Background technique [0002] With the increasing depletion of global petrochemical resources, biodiesel, as one of the alternative energy sources, is favored. However, as the output of biodiesel continues to rise, the output of its by-product glycerol has also continued to increase. At present, because glycerin is mainly used in the pharmaceutical and cosmetic industries, the demand is very limited. Therefore, the research of preparing high value-added chemicals from glycerin has received great attention. Acrolein is an important fine chemical intermediate, mainly used in the production of pesticide insecticide imidacloprid, pharmaceutical antitumor drug dibromopropionaldehyde, feed additive methionine, fungicide glutaraldehyde; acrolein can be oxidized to produce acrylic acid, an...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C45/52C07C47/22
Inventor 丁建飞朱烨楠马田林邵荣许伟
Owner YANCHENG INST OF TECH
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