Polyacid @aluminum oxide composite catalytic material and preparing method thereof

A technology of composite catalytic materials and alumina, which is applied in the application field of catalytic thioether oxidation reaction, can solve problems such as not easy to be affected by active components, loss of multi-acid, increase of active components, etc., to achieve the reaction time and the amount of hydrogen peroxide The effect of reducing, good catalytic performance and improving cycle stability

Active Publication Date: 2016-07-06
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But these two kinds of methods all have its shortcoming: the multi-acid-based supported catalyst synthesized by the method of electrostatic interaction, the multi-acid is easy to lose from the carrier in the liquid phase reaction; the multi-acid synthesized by the multi-acid roasting Supported catalysts will form a variety of active components, which makes it more difficult to identify the active components in the catalytic reaction, and it is not easy to understand the impact of each active component on the reaction

Method used

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  • Polyacid @aluminum oxide composite catalytic material and preparing method thereof
  • Polyacid @aluminum oxide composite catalytic material and preparing method thereof
  • Polyacid @aluminum oxide composite catalytic material and preparing method thereof

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Embodiment 1

[0020] 1) Calcining γ-alumina balls at 500°C for 22 hours and cooling to room temperature;

[0021] 2) Add 4g of Na 12 [α-P 2 W 15 o 56 ]·24H 2 O and 20g of calcined γ-alumina balls were dispersed in 500mL of water, the pH value of the solution was adjusted to 1.5 with hydrochloric acid, the magnetic stirring reaction was performed at room temperature for 2 hours, the temperature was raised to 80°C and the magnetic stirring reaction was continued for 2 hours, filtered, and 2mol / L lithium chloride solution to wash the product three times, and vacuum-dry at 60° C. for 12 hours to obtain a multi-acid alumina nanocomposite catalytic material.

[0022] The multi-acid alumina nanocomposite catalytic material prepared above is used to catalyze the oxidation reaction of thioether: weigh 2.5 μmol of the synthesized polyacid alumina nanocomposite catalytic material in a round bottom flask, then successively add 1mmol sulfide anisole, Add 1mmol hydrogen peroxide and 200μL methanol ...

Embodiment 2

[0026] 1) Calcining gamma-alumina balls at 500°C for 25 hours and cooling to room temperature;

[0027] 2) Add 4g of Na 8 H[A-PW 9 o 34 ]·7H 2 O and 20 g of calcined γ-alumina balls were dispersed in 500 mL of water, and the pH value of the solution was adjusted to 0.5 with hydrochloric acid. The reaction was carried out under magnetic stirring at room temperature for 3 hours, and the temperature was raised to 85°C to continue the magnetic stirring reaction for 2 hours. The product was washed three times, and vacuum-dried at 60° C. for 12 hours to obtain a multi-acid alumina nanocomposite catalytic material.

[0028] The multi-acid alumina nano-composite catalytic material prepared above is used to catalyze the oxidation reaction of thioether: weigh 2.5 μmol of the synthesized multi-acid alumina nano-composite catalytic material in a round bottom flask, then successively add 1 mmol sulfide anisole, Add 1mmol hydrogen peroxide and 200μL methanol into a round-bottomed flask,...

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Abstract

The invention discloses a polyacid@aluminum oxide composite catalytic material and a preparing and activated gamma-aluminum oxide balls are compounded under the acidic condition, the surface of aluminum oxide is modified with polyoxometallate molecules in a covalent bond mode, and highly-stable immobilization and uniform loading of polyoxometallate on aluminum oxide are achieved under the premise of maintaining the nuclear cluster integrity of polyoxometallate.Selected polyoxometallate Na12[alpha-P2W15O56] and Na8H[A-PW9O34] have a high oxidation state and thus have excellent oxidation performance, and when the composite catalytic material of polyoxometallate is applied to a catalytic sulfur ether oxidation reaction, good catalytic activity and circulation stability are achieved.Compared with reported polyacid and aluminum oxide nano-composite catalytic materials and pure polyacid, the synthesized composite catalytic material remarkably improves the circulation stability of the sulfur ether oxidation reaction, shortens the reaction time, reduces the dosage of hydrogen peroxide and maintains a good conversion rate and selectivity when serving as a catalyst of the sulfur ether oxidation reaction.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic composite materials, in particular to a preparation method of a series of polyacid and alumina composite catalytic materials and its application in catalyzing sulfide oxidation reaction. Background technique [0002] Polyacid compounds are a class of multimetal oxides containing V, Mo, W, Nb and other metals, which have high oxidation states due to their unique structures, making them widely used in the field of catalytic oxidation. However, polyacids have high solubility in solution and are easy to crystallize out of solution. This limits the application of polyacids in industrial reactions. Therefore, the study of heterogeneous polyacid catalysts has become an important direction to improve the recovery, selectivity and thermal stability of polyacid-based catalysts. [0003] Immobilization and curing are two widely used methods for the synthesis of polyacid-based heterogeneous...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J27/188C07C315/02C07C317/14C07C317/12
CPCB01J27/188C07C315/02C07C317/14C07C317/12Y02P20/50
Inventor 宋宇飞洪兰兰陈伟
Owner BEIJING UNIV OF CHEM TECH
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