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Molybdenyl acetylacetonate solid catalyst used for alkene epoxidation reaction and preparation method thereof

A technology of molybdenum acetylacetonate and solid catalyst, which is applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc. It is easy to block the pores, and the single loading of active components is not high, so as to achieve the effects of simple filtration, recovery and reuse, reduced catalytic activity, and simple preparation.

Active Publication Date: 2015-09-09
湖州优研知识产权服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of these complexes lead to homogeneous catalytic systems, and the catalysts are difficult to recover and reuse
The traditional solution is to immobilize organometallic compounds on carriers such as molecular sieves and activated carbon through coupling agents (such as triethoxysilane, etc.) to prepare supported catalysts, but the reported loading methods are not only cumbersome to prepare , the single loading of the active component is not high, and there are disadvantages such as the active component is easy to block the pores and dissolve
[0004] In order to solve the above problems, the present invention adopts free radical polymerization method to prepare organic polymer immobilized molybdenum acetylacetonate solid catalyst to catalyze olefin epoxidation reaction, and this method has not been reported yet.

Method used

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  • Molybdenyl acetylacetonate solid catalyst used for alkene epoxidation reaction and preparation method thereof
  • Molybdenyl acetylacetonate solid catalyst used for alkene epoxidation reaction and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0014] In a 100mL round bottom flask, add 0.05mol of divinylbenzene and 0.05mol of allylamine into 50mL of ethanol solvent, add 0.18g of initiator azobisisobutyronitrile AIBN, stir at 80°C for 24h, and filter out The solid product was washed three times with ethanol, and dried in vacuum at 60°C for 10 hours to obtain the organic polymer DVB-NH 2 , 0.02mol of DVB-NH 2 Add 0.01mol oxymolybdenum acetylacetonate into 50mL ethanol solvent, stir magnetically at 80°C for 48h, filter and separate the solid product, wash with ethanol three times, and dry under vacuum at 60°C for 10h to obtain the solid catalyst DVB-NH 2 -MoO 2 (acac) 2 .

Embodiment 2

[0016] In a 50mL round bottom flask, add 0.01mol cyclooctene, 0.02mol tert-butyl hydroperoxide and 20mL dichloromethane, then add 0.2g solid catalyst DVB-NH 2 -MoO 2 (acac) 2 , at a reaction temperature of 70° C., stirred for 4 hours, and the chromatographic analysis showed that the conversion rate of cyclooctene was 95%, and the selectivity of epoxy cyclooctane was 98%.

Embodiment 3

[0018] In a 50mL round bottom flask, add 0.01mol cycloethylene, 0.02mol tert-butyl hydroperoxide and 20mL dichloromethane, then add 0.2g solid catalyst DVB-NH 2 -MoO 2 (acac) 2 , at a reaction temperature of 70° C., stirred for 4 hours, and the chromatographic analysis showed that the conversion rate of cycloethylene was 89%, and the selectivity of epoxycyclohexane was 94%.

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Abstract

The invention discloses a molybdenyl acetylacetonate solid catalyst used for an alkene epoxidation reaction and a preparation method thereof. According to the invention, divinyl benzene and allyl amine are subjected to a free radical polymerization to obtain an organic macromolecule polymer, then a molybdenyl acetylacetonate organic ligand and amino on a polymer frame are subjected to a chemical bond effect to prepare the loaded molybdenyl acetylacetonate solid catalyst. The catalyst preparation method has the advantages of simple and easy operation, high catalysis efficiency, repeatedly usable performance and reduced production cost, and is expected to become a cleaning epoxidation technology route having competitiveness.

Description

technical field [0001] The invention relates to a preparation method of a novel solid catalyst for olefin epoxidation reaction. The solid epoxidation catalyst DVB-NH is prepared by using an organic polymer to support molybdenum acetylacetonate 2 -MoO 2 (acac) 2 , belonging to the field of fine organic chemical technology. Background technique [0002] The epoxidation reaction of olefins has been widely studied both in theoretical exploration and in actual production, because epoxides, as an important class of organic chemical intermediates, have been widely used in fine organic synthesis and organic chemical processes. In order to overcome the shortcomings and shortcomings of a series of equipment corrosion and high energy consumption brought about by the traditional peroxycarboxylic acid method to catalyze olefin epoxidation, or the industrial application limitations associated with the use of noble metals such as Ag as catalysts, in recent years, people will More attent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07D303/04C07D301/19
Inventor 冷炎卢丹蒋平平
Owner 湖州优研知识产权服务有限公司