Method for preparing magnetic composite biobased supported phosphotungstic acid catalyst

A magnetic composite microsphere, bio-based technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of composite microsphere carrier damage and unfavorable immobilization And other problems, to achieve the effect of easy functional modification, not easy to leak, good magnetic effect

Inactive Publication Date: 2017-11-07
NORTHEAST FORESTRY UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method of co-precipitation to prepare magnetic ferroferric oxide requires severe mechanical stirring during the preparation process, and mechanical stirring will cause serious damage to the composite microsphere carrier, which is not conducive to the impact of graphene oxide / cellulose composite microspheres on subsequent experiments. Immobilization of phosphotungstic acid

Method used

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  • Method for preparing magnetic composite biobased supported phosphotungstic acid catalyst
  • Method for preparing magnetic composite biobased supported phosphotungstic acid catalyst
  • Method for preparing magnetic composite biobased supported phosphotungstic acid catalyst

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Effect test

Embodiment 1

[0026] Put 5g of cellulose into 66g of ionic liquid to dissolve, add 40mL (1mg / 1.6mL) graphene oxide solution and mix evenly, mechanically stir in the transformer oil by high-speed electric stirring equipment, and immobilize into balls by reverse-phase suspension technology, After repeated washing with absolute ethanol and 4% hydrochloric acid, the obtained composite mesoporous microspheres were dried for future use. Next, put 5g of dry composite mesoporous microspheres into 5mL of epichlorohydrin and 10mL of 3mol / L sodium hydroxide solution, react on a shaking table at 25°C for 8h, and wash and filter the microspheres repeatedly to the pH of the filtrate after the reaction To be neutral, disperse the microspheres into an aqueous solution of triethylenetetramine and sodium carbonate and react in a water bath at 50°C for 8h. After the reaction is finished, it is washed with deionized water to remove the remaining reaction liquid, and the obtained amine-functionalized composite ...

Embodiment 2

[0028] Open the negative pressure valve ⑨, start the negative pressure pump ⑧, make the negative pressure in the tank ④ reach -0.08~-0.09MPa, open the sampling valve ②, and remove 3.81g ferrous chloride, 9.75g ferric chloride and 200mL Ionized water is sucked into the tank body ④, the sampling valve ② is closed, the nitrogen valve is opened, and the ferric chloride and ferric chloride are fully dissolved in the deionized water through the cavitation generated by the negative pressure equipment, and the Fe in the mixed solution is 3+ with Fe 2+ The molar ratio is 2:1, close the nitrogen valve, open the injection valve ②, inhale 5g of modified composite microspheres into the tank ④, close the injection valve ②, open the nitrogen valve for 1h, and keep the tank ④ at the same time. Negative pressure is still -0.08~-0.09MPa, close the nitrogen valve, open the sampling valve ② Inhale ammonia water until the pH of the mixture is 9, heat the equipment to 60°C through the heating syste...

Embodiment 3

[0030]Dissolve 2g of phosphotungstic acid in 20mL of absolute ethanol medium, add 2g of amine-functionalized magnetic composite microspheres, control the temperature at 60°C, and immobilize for 2 hours, stop stirring after the reaction is complete, and filter off the excess reaction solution , Dry the catalysts that are used in many fields such as catalyzed organic reactions, medicinal chemistry and magnetic materials.

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Abstract

The invention discloses a method for preparing a magnetic composite biobased supported phosphotungstic acid catalyst, aiming to provide a method which is high in supporting ratio and good in stability, and is economic and safe for preparing a magnetic composite biobased supported phosphotungstic acid catalyst. The magnetic composite biobased supported phosphotungstic acid catalyst is made by performing thermosetting through adoption of reverse suspension technology to form graphene oxide / cellulose composite microspheres; performing amino functional modification to the composite microspheres through a chemical grafting means; preparing nanometer-Fe3O4-modified magnetic composite microspheres through adoption of negative-pressure cavitation auxiliary coprecipitation technology; and using intermolecular ionic bonds and Van der Waals force on porous structured surfaces of the composite microspheres. The prepared catalyst is good in catalytic activity and magnetic effect and high in mechanical strength, can be recycled for several times, and is widely applied to various catalytic fields.

Description

technical field [0001] The invention relates to a method for preparing a magnetic composite bio-based immobilized phosphotungstic acid catalyst, belonging to the technical field of catalysts. Background technique [0002] Phosphotungstic acid (H 3 PW 12 o 40 ·nH 2 O, HPW) is an oxygen-containing polyacid composed of a heteroatom P and a coordination atom W in a certain structure through an oxygen atom coordination bridge, which has strong acidity (stronger than the traditional homogeneous liquid acid, such as H 2 SO 4 ), high catalytic activity and stability. Therefore, the use of phosphotungstic acid as a catalyst is being rapidly developed and widely used in catalytic organic reactions, medicinal chemistry, solute liquid crystals, high proton conductors and nonlinear optical materials. However, the phosphotungstic acid catalyst is expensive, has a small surface area, and is difficult to separate from the reaction system. Therefore, immobilizing it on a carrier with a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/34
CPCB01J31/34
Inventor 付玉杰王希清李天凤焦骄刘天舒王微姚丽萍
Owner NORTHEAST FORESTRY UNIVERSITY
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