Preparation method of magnetic heteropoly acid-graphene composite catalytic material

A graphene composite and catalytic material technology, which is applied in the field of preparation of new heteropolyacid-graphene composite catalytic materials, can solve the problems of small specific surface area, low pollution rate and difficult recovery of heteropolyacid, and achieve uniform appearance, The effect of low preparation cost and simple equipment requirements

Active Publication Date: 2017-01-04
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Heteropoly acid, a green, non-toxic, non-corrosive and environmentally friendly catalyst, has been successfully applied in a variety of organic reactions, such as: esterification etherification, condensation reaction, alkylation, hydration dehydration and polymerization, etc. The reaction presents many advantages such as high reactivity, low corrosion, and low pollution rate, but the application of heteropolyacids in the field of catalysis is limited due to the small specific surface area of ​​heteropolyacids and difficulties in recycling.

Method used

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  • Preparation method of magnetic heteropoly acid-graphene composite catalytic material
  • Preparation method of magnetic heteropoly acid-graphene composite catalytic material
  • Preparation method of magnetic heteropoly acid-graphene composite catalytic material

Examples

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Effect test

Embodiment 1

[0027] 1) Preparation of magnetic carrier material: ultrasonically dissolve 40 mg of graphene oxide in 25 ml of distilled aqueous solution, stir for 30 min, then add 0.68 g of ferrous sulfate to the graphene solution, then add 0.20 g of sodium hydroxide, 1.50 g of polyvinylpyrrolidone g and urea 1.80g. The above solution was transferred to a reaction kettle, and the hydrothermal reaction was carried out at 180° C. for 6 hours. After the reaction, the product was filtered, washed, dried at 60° C. and the solid was collected to obtain a magnetic carrier material.

[0028] 2) Preparation of heteropoly acid-Na 12 [WZn 3 (ZnW 9 o 34 ) 2 ]Materials: Dissolve 6.35g of sodium tungstate in 50ml of distilled water, heat and stir at 85°C until completely dissolved; dissolve 1.50g of zinc nitrate in 5ml of distilled water, add to the above solution, condense and reflux at 85°C for 2 hours After the reaction is finished, filter and collect the filtrate, wait for crystallization, and o...

Embodiment 2

[0031] 1) Preparation of magnetic carrier material: ultrasonically dissolve 80 mg of graphene oxide in 50 ml of distilled aqueous solution, stir for 30 min; then add 1.36 g of ferrous sulfate into the graphene solution, then add 0.40 g of sodium hydroxide, 3.00 g of polyvinylpyrrolidone g and urea 3.60g. The above solution was transferred to a reaction kettle, and the hydrothermal reaction was carried out at 180° C. for 6 hours. After the reaction, the product was filtered, washed, dried at 60° C. and the solid was collected to obtain a magnetic carrier material.

[0032] 2) Preparation of heteropoly acid-Na 12 [WZn 3 (ZnW 9 o 34 ) 2 ] Material: Dissolve 12.70g of sodium tungstate in 100ml of distilled water, heat and stir at 85°C until completely dissolved; dissolve 3.00g of zinc nitrate in 10ml of distilled water, add to the above solution, condense and reflux at 85°C for 2 hours After the reaction is finished, filter and collect the filtrate, wait for crystallization, ...

Embodiment 3

[0035] 1) Preparation of magnetic carrier material: ultrasonically dissolve 160 mg of graphene oxide in 100 ml of distilled aqueous solution, stir for 30 min, then add 2.72 g of ferrous sulfate to the graphene solution, then add 0.80 g of sodium hydroxide, 6.00 g of polyvinylpyrrolidone g and urea 7.20g. The above solution was transferred to a reaction kettle, and the hydrothermal reaction was carried out at 180° C. for 6 hours. After the reaction, the product was filtered, washed, dried at 60° C. and the solid was collected to obtain a magnetic carrier material.

[0036] 2) Preparation of heteropoly acid-Na 12 [WZn 3 (ZnW 9 o 34 ) 2 ]Materials: Dissolve 25.40g of sodium tungstate in 200ml of distilled water, heat and stir at 85°C until completely dissolved; dissolve 6.00g of zinc nitrate in 20ml of distilled water, add to the above solution, condense and reflux at 85°C for 2 hours After the reaction is finished, filter and collect the filtrate, wait for crystallization, ...

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Abstract

The invention provides a preparation method of a magnetic heteropoly acid-graphene composite catalytic material and belongs to the field of chemical catalytic materials.Ferrous sulfate, sodium hydroxide, polyvinylpyrrolidone and urea are mixed with a graphene solution, and hydrothermal reaction is performed to obtain a magnetic carrier material; the magnetic carrier material is dissolved in distilled water under ultrasonic conditions, then hexadecyl trimethyl ammonium bromide and a heteropoly acid material are added, magnetic separation is performed to obtain a solid after mixing, and washing and drying are performed to obtain themagnetic heteropoly acid composite catalytic material. The method is simple, the raw materials are easy to obtain, the prepared material isuniform in magnetic particle morphology and uniform in distribution, and the magnetic carrier has a larger specific surface area.

Description

technical field [0001] The invention belongs to the field of chemical catalytic materials, and in particular relates to a preparation method of a novel heteropolyacid-graphene composite catalytic material with magnetic properties. Background technique [0002] With the rapid development of nanotechnology, magnetic nanoparticles have been extensively studied and widely used in physics, medicine, biology, and material science. Compared with magnetic nanoparticles, magnetic composite nanoparticles have better biocompatibility, easy functionalization, better physical and chemical properties, and are more conducive to their wide application. [0003] Heteropoly acid is a kind of solid acid, which has unique oxidation-reduction properties, acidity and dual functions, and can show strong catalytic activity in many chemical reactions. Heteropoly acid, a green, non-toxic, non-corrosive and environmentally friendly catalyst, has been successfully applied in a variety of organic react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/16B01J23/888
CPCB01J23/888B01J27/188B01J35/0033
Inventor 倪鲁彬李欢梁大帅赵钢筋吴常浪孙聪喻拯东李逸
Owner YANGZHOU UNIV
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