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Au@MnPS catalyst as well as preparation method and use thereof

A catalyst and application technology, applied in the field of Au@MnPS catalyst and its preparation and application, can solve the problem of no olefin oxidation, etc., and achieve the effect of good conversion rate and selectivity, and mild conditions

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

AI Technical Summary

Problems solved by technology

However, the current research on Au@MOFs basically only focuses on the oxidation of alcohols, and there is basically no research on the oxidation of alkenes.

Method used

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  • Au@MnPS catalyst as well as preparation method and use thereof
  • Au@MnPS catalyst as well as preparation method and use thereof
  • Au@MnPS catalyst as well as preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Preparation of Au@MnPS catalyst:

[0025] 3. Dissolve 8625g of vanillin in 50 mL of propionic acid, reflux at 141°C, slowly add 1.3 mL of pyrrole dropwise, and react for 45 minutes. Cool to room temperature, filter with suction, and wash several times with anhydrous methanol. The obtained purple-red solid was dried at 110° C. for 2 hours; 0.2415 g of the obtained porphyrin and 1.2255 g of manganese acetate were dissolved in DMF and put into a hydrothermal synthesis kettle. After reacting at 180° C. for 48 h, cool to room temperature, filter with suction, and wash with deionized water to obtain a black block of MnPS solid, which is ground to powder. Get the black solid 0.5g that above-mentioned steps obtains, add urea 0.9g in the there-necked flask, add different amounts of chloroauric acid solution (HAuCl 4 4H 2 O, the concentration is 0.1g / L), diluted to 30mL with deionized water. After stirring and reflux at 80°C for 6h, add 30mL of commercially available formalde...

Embodiment 2

[0029] Catalyst activity evaluation. Gold content 2% Au@MnPS catalyst 0.10 g was placed in a PTFE-lined autoclave (volume = 20 mL), 0.8215 g of cyclohexene, solvent acetonitrile 10 mL, TBHP initiator 5 drops, and molecular oxygen as an oxidant at 1 MPa The reaction was stirred at 80°C for 20 hours under pressure. The conversion rate that obtains cyclohexene oxidation is 45.047%, the selectivity of epoxy cyclohexane is 68.406%, the selectivity of cyclohexenol is 12.502%, the selectivity of cyclohexenone is 12.675%, and the selectivity of o-cyclohexanedi The selectivity of alcohol is 6.416%.

Embodiment 3

[0031] Catalyst activity evaluation. A gold content of 2% Au@MnPS catalyst 0.10 g was used for the reaction. 0.8215g of cyclohexene, solvent acetonitrile 10mL, 5 drops of TBHP initiator, and molecular oxygen as an oxidizing agent were stirred and reacted at 80° C. for 5 hours under a pressure of 1 MPa. The conversion rate that obtains cyclohexene oxidation is 39.667%, the selectivity of epoxy cyclohexane is 52.966%, the selectivity of cyclohexenol is 9.566%, the selectivity of cyclohexenone is 10.827%, and the selectivity of o-cyclohexanedi The selectivity of alcohol is 26.641%.

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PUM

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Abstract

The invention discloses an Au@MnPS catalyst as well as a preparation method and use thereof. According to the preparation method, MnPS is prepared and is loaded with nanogold to form the Au@MnPS catalyst, wherein MnPS is used as a carrier of the catalyst, and a manganese porphyrin structure in Au and MnPS is taken as a main active component of the catalyst and has relatively high loading efficiency and relatively good dispersion degree. The catalyst provided by the invention has the characteristics of high activity and good selectivity in the preparation of cyclohexene oxide from cyclohexene through epoxidation and meets the requirements of industrial production.

Description

technical field [0001] The present invention relates to a kind of Au@MnPS 3 The preparation method of the catalyst and its application in the epoxidation of cyclohexene. Background technique [0002] Selective oxidation of cyclohexene is an important process for the synthesis of various high value-added intermediates cyclohexenol, cyclohexenone and epoxycyclohexane. Because the cyclohexene molecule contains an unsaturated C=C double bond and multiple active α-H atoms that are prone to oxidation reactions, the selectivity of the oxidation reaction is poor and the products are complex. Academia and industry have been looking for The catalyst with high activity and high selectivity under mild conditions is used for catalytic oxidation of cyclohexene. Heterogeneous catalysts have the advantages of easy separation from products and easy recycling, and are one of the main research directions of green catalytic processes. [0003] New heterogeneous catalysts cover many direction...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J31/26C07D301/06C07D303/04
CPCB01J31/1691B01J31/183B01J31/26B01J2231/72B01J2531/025B01J2531/72C07D301/06C07D303/04
Inventor 朱明乔刘懿陈新志陈亨权江勤
Owner ZHEJIANG UNIV
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