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Spherical V-MCM-48 catalyst for hydrogen peroxide selective oxidation of phenylethylene oxide and method

A V-MCM-48, catalyst technology, applied in the field of hydrogen peroxide selective styrene oxide, to achieve the effect of changing distribution, high activity and low cost

Active Publication Date: 2014-06-25
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction needs to be carried out in a closed reactor; at the same time, only one main substance of benzaldehyde is obtained in this patent, and styrene oxide is not involved

Method used

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  • Spherical V-MCM-48 catalyst for hydrogen peroxide selective oxidation of phenylethylene oxide and method
  • Spherical V-MCM-48 catalyst for hydrogen peroxide selective oxidation of phenylethylene oxide and method
  • Spherical V-MCM-48 catalyst for hydrogen peroxide selective oxidation of phenylethylene oxide and method

Examples

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Effect test

example 1

[0018] [Example 1] catalyst synthesis

[0019] 1.0125g of cetyltrimethylammonium bromide was dissolved in 69.1ml of deionized water, 24.2ml of ethanol and 6.3ml of ammonia (NH 3 In the mixed solution whose mass concentration is 27%), it is recorded as solution A. At the same time, 0.0108 g of ammonium metavanadate was dissolved in 10 ml of deionized water, which was recorded as solution B. Slowly add B to A, followed by 2.1 ml tetraethylorthosilicate. After stirring for 1 h, the obtained gel was put into a reactor for hydrothermal reaction at 100° C. for 24 h. The solid obtained after centrifugation was washed, dried, and calcined in a muffle furnace at 550° C. for 6 h to remove the surfactant, and the obtained catalyst was designated as C1. The XRD, SEM and low-temperature nitrogen adsorption diagrams of sample C1 are detailed in Figure 1 ~ Figure 3 , it can be seen from the XRD pattern that this sample has a narrow peak at 2θ of 211 and three small peaks at 2θ of 3.0-5....

example 2

[0020] [Example 2] Synthesis of Catalyst

[0021] Dissolve 0.3355g nonadecyltrimethylammonium chloride in 69.1ml deionized water, 49.3ml propanol and 6.3ml ammonia water (NH 3 In the mixed solution whose mass concentration is 27%), it is recorded as solution A. At the same time, 0.216 g of ammonium metavanadate was dissolved in 10 ml of deionized water, which was recorded as solution B. Slowly add B to A, followed by 2.1 ml tetraethylorthosilicate. After stirring for 2 hours, the obtained gel was put into a reactor for hydrothermal reaction at 40° C. for 24 hours. The solid obtained after centrifugation was washed, dried, and calcined in a muffle furnace at 500° C. for 5 h to remove the surfactant, and the obtained catalyst was designated as C2. The catalyst has a spherical shape, and the diameter of the sphere is 0.1-1 μm.

example 3

[0022] [Example 3] Synthesis of Catalyst

[0023] 0.7013g of octaalkyltrimethylammonium bromide was dissolved in 62.1ml of deionized water, 21.9ml of ethylene glycol and 4.5ml of ammonia (NH 3 In the mixed solution whose mass concentration is 30%), it is recorded as solution A. At the same time, 0.0432 g of ammonium metavanadate was dissolved in 10 ml of deionized water, which was recorded as solution B. Slowly add B to A, followed by 2.1 ml tetraethylorthosilicate. After stirring for 3 hours, the obtained gel was put into a reactor for hydrothermal reaction at 80° C. for 12 hours. The solid obtained after centrifugation was washed, dried, and calcined in a muffle furnace at 600° C. for 7 h to remove the surfactant, and the obtained catalyst was designated as C3. The catalyst has a spherical shape, and the diameter of the sphere is 0.1-1 μm.

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Abstract

The invention relates to a spherical V-MCM-48 catalyst, which is produced with the following method: a certain amount of ammonium metavanadate is dissolved in a small amount of water, the aqueous solution is added to mixed solution which contains a surface active agent, alcohol and ammonia water, after mixing and dissolving, a silicon source is added, gel is obtained through reaction, and then the catalyst is obtained by washing, separating, drying and removing surface active agent after aging on the hydrothermal condition. The invention further provides a method for hydrogen peroxide selective oxidation of phenylethylene oxide by using the catalyst. The method has the advantages of using the catalyst to obtain high styrene conversion rate and product selectivity and being capable of changing yield rate of reaction product of benzaldehyde and styrene oxide by adjusting potential of hydrogen (pH) of reaction liquid.

Description

technical field [0001] The invention relates to a vanadium-doped V-MCM-48 catalyst with a spherical shape and a method for selectively oxidizing styrene with hydrogen peroxide using the catalyst. Background technique [0002] M41s mesoporous material has the characteristics of large specific surface area, regular and adjustable pore structure, etc., and has great potential application value in the fields of catalysis, medicine, environmental protection, and adsorption. As one of the important members of the M41s family, the MCM-48 material has a special bicontinuous three-dimensional cubic channel structure, which makes its performance better than that of the one-dimensional similar mesoporous molecular sieves. MCM-48 is usually synthesized under long-term hydrothermal conditions using high-concentration surfactants or mixed surfactants, which consumes a lot of energy and costs. Pure MCM-48 has a narrow application range, and the introduction of metal ions will establish ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/78B01J35/08C07D303/04C07D301/12
Inventor 孔岩许晓颖孙庆林时晓波
Owner NANJING TECH UNIV
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