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Nickel-based catalyst, preparation method and application thereof, and method for preparing organic ester through catalytic oxidation of organic ketone

A technology of nickel-based catalysts and nickel oxides, which is applied in organic chemistry, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as easy-to-corrosion equipment, difficult organic acid recovery, and separation difficulties, so as to improve the reaction yield. High efficiency and selectivity, suitable for large-scale production, cheap and easy-to-obtain raw materials

Active Publication Date: 2020-08-04
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These peroxides have good oxidation activity as oxidants, but there are following disadvantages: (1) homogeneous reaction system causes separation difficulties, and the recovery of organic acids is also difficult; (2) residual peroxyacids and by-products are easy to corrode equipment, pollute the environment, and easily lead to the polymerization of organic esters to form oligomers during vacuum distillation; (3) peroxyacids have great potential safety hazards in the process of preparation, transportation and use
However, mononuclear metalloporphyrins or oxygen-containing binuclear metalloporphyrins are easily deactivated as catalysts, which limits their application in Baeyer-Villiger reactions.

Method used

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preparation example Construction

[0034] The present invention provides the preparation method of nickel-based catalyst described in above-mentioned technical scheme, (1) when described active component is transition metal-nickel composite oxide, the preparation method of described nickel-based catalyst comprises the following steps:

[0035] Mixing soluble transition metal salts, soluble nickel salts, and carbon-containing raw materials, and performing programmed roasting under a protective atmosphere to obtain a precursor; the carbon-containing raw materials include carbon nanotubes, activated carbon or melamine;

[0036] The precursor and H 2 o 2 The aqueous solution is mixed and dried to obtain a nickel-based catalyst;

[0037] (II) when described active component is nickel oxide, the preparation method of described nickel-based catalyst comprises the following steps:

[0038] Mix soluble nickel salt and carbon-containing raw materials, and perform programmed roasting under a protective atmosphere to obt...

Embodiment 1

[0076] Grind and mix 100mmol zinc chloride, 200mmol nickel chloride hexahydrate and 500mmol melamine evenly, place the resulting mixed powder in a crucible, and raise the temperature from room temperature to 550°C at a heating rate of 2.5°C / min in a nitrogen atmosphere After the last calcination for 1 hour, after naturally lowering to room temperature, the temperature was raised from room temperature to 750 ℃ ​​at a heating rate of 10 ℃ / min, then the second calcination was performed for 1 hour, and then the temperature was naturally lowered to room temperature to obtain the precursor;

[0077] 20 mL of 15 wt% H was added dropwise to 1 g of the precursor 2 o 2 aqueous solution, stirred and mixed for 60 minutes, dried at 80°C for 12 hours, and then ground to obtain a nickel-based catalyst (abbreviated as ZnNi 2 o 3 -C 3 N 4 , particle size of 40 to 80 mesh).

Embodiment 2

[0079] Prepare nickel-based catalyst according to the method of embodiment 1, and the difference with embodiment 1 is, add 100mmol zinc chloride, 500mmol nickel chloride hexahydrate, obtain nickel-based catalyst (abbreviated as ZnNi 5 o 6 -C 3 N 4 ).

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Abstract

The invention provides a nickel-based catalyst, a preparation method and an application thereof and a method for preparing organic ester through a catalytic oxidation of organic ketone, which relate to the technical field of organic ester preparation. The nickel-based catalyst provided by the invention comprises a carrier and active components loaded on pore channels and the surface of the carrier, wherein the carrier comprises carbon nanotubes, activated carbon or nitrogen-doped carbon; wherein the active component comprises a nickel oxide or a transition metal-nickel composite oxide. In theinvention, the nickel-based catalyst is used in the process of preparing the organic ester by the catalytic oxidation of the organic ketone, nickel can efficiently activate oxygen to generate peroxy radicals so as to oxidize the aldehyde oxidant into peroxy acid, and the peroxy acid continues to oxidize the organic ketone to generate the organic ester; the transition metal can activate carbonyl, so that peroxy acid attacks the activated carbonyl more easily, and the activation energy of the reaction is reduced; the carrier has a large number of pore structures, so that more metal active sitesare exposed, the pore structures can stabilize and store free radicals, and the conversion rate of organic ketone is increased.

Description

technical field [0001] The invention relates to the technical field of preparation of organic esters, in particular to a nickel-based catalyst, a preparation method and application thereof, and a method for preparing organic esters by catalytic oxidation of organic ketones. Background technique [0002] The selective oxidation of organic ketones to the corresponding organic esters is an important industrial process. The Baeyer-Villiger reaction (abbreviated as B-V reaction) is a type of oxidation reaction that oxidizes organic ketones into corresponding organic esters, also known as Baeyer–Villiger rearrangement. This process is generally carried out by peroxyacid oxidation, H 2 o 2 Oxidation method, molecular oxygen oxidation method and biological oxidation method. [0003] Commonly used organic peroxyacids include peroxyformic acid, peroxyacetic acid, peroxypropionic acid, monoperoxyphthalic acid and m-chloroperoxybenzoic acid (m-CPBA), and commonly used inorganic perox...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07D313/04C07D309/30
CPCB01J27/24C07D309/30C07D313/04
Inventor 李建辉马旭飞钟越李伟鹏张立忠张俊孙毅飞
Owner XIAMEN UNIV