Method of preparing aldehyde or ketone by alcohol liquid phase selection oxidization accelerated by micro-wave

A technology of phase selection and alcohol solution, which is applied in the direction of oxidation preparation of carbonyl compounds, chemical instruments and methods, chemical/physical processes, etc., can solve environmental pollution, toxicity, unfavorable practical application and other problems, and achieve the effect of high atom economy

Inactive Publication Date: 2007-10-17
FUDAN UNIV
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Problems solved by technology

But this system adopts trioctyl methyl ammonium hydrogensulfate as the raw material of phase transfer catalyst, and the quaternary ammonium salt has no industrial production yet, and the prepar

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-8

[0012] Examples 1-8: Experimental results of catalytic selective oxidation of alcohols to aldehydes and ketones in the presence of different additives. Experimental conditions: 100mL flask, the catalyst is sodium tungstate dihydrate (Na 2 WO 4 2H 2 O, 2mmol), 100mmol benzyl alcohol, 15.3mL hydrogen peroxide (30%), react at 70°C for 2h. The reaction results are shown in Table 1.

[0013] Reality

[0014] a The ratio of the auxiliary agent to the amount of tungsten element in the tungsten-containing catalyst is 1:1.

Embodiment 9-15

[0017] Examples 9-15: Experimental results of selective oxidation of alcohols to aldehydes and ketones catalyzed by different catalysts. Experimental conditions: 100mL flask, additives are oxalic acid, 100mmol benzyl alcohol, 15.3mL hydrogen peroxide (30%), react at 70°C for 2h, microwave power is 600W. The reaction results are shown in Table 3.

[0018] Reality

Embodiment 16-23

[0019] Examples 16-23: Experimental results with different alcohols on the same catalyst. Experimental conditions: 100mL flask, the catalyst is sodium tungstate dihydrate (Na 2 WO 4 2H 2 O), auxiliary agent is oxalic acid (2mmol), 100mmol alcohol, hydrogen peroxide (30%) 15.3mL, 70 ℃ reaction 2h, microwave power is 600W. The reaction results are shown in Table 4.

[0020] example

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PUM

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Abstract

The present invention belongs to technology field for preparing aldehyde or ketone by oxidizing alcohol, particularly which is microwave-promoted method for preparing aldehyde or ketone by alcohol liquid-phase selective catalytic oxidation. The present invention prepares aldehyde or ketone by catalytic oxidation of alcohol under microwave irradiation, which takes sodium tungstate and tungstic heteropolyacid salts as catalyst, takes bidentate ligand containing nitrogen and oxygen as additive and takes hydrogen peroxide as preparing oxidant. The catalyst system used in the present invention uses very small quantity compared with raw materials alcohol and oxidant, and it has high atomic economy and will not pollutes environment.There is not any organic solvent and phase transfer catalyst used in entire procedure, which is easy to separate for obtaining product by simple operational, whose reaction conditional is mild and easy to operate. The present invention is suitable for the reaction for generating aldehyde by oxygenizing various alcohols which include aliphatic alcohol, ester cyclitol, aromatic alcohol and diatomic alcohol, and which have high conversion rate to alcoholic and high selectivity to aldehyde or ketone.

Description

technical field [0001] The invention belongs to the technical field of producing aldehydes and ketones by oxidation of alcohols, and in particular relates to a method for preparing aldehydes or ketones by high-efficiency liquid-phase oxidation of alcohols by using microwave irradiation as a process strengthening means. technical background [0002] The selective oxidation of alcohols to the corresponding carbonyl compounds is an important chemical process in the field of organic synthetic chemistry. This process is widely used in fine chemical industries such as pharmaceuticals, fertilizers, and spices. The traditional process methods mostly use chemical doses of oxidants, but a large amount of waste and by-products will be generated during use, which seriously pollutes the environment. Hydrogen peroxide is an ideal cleaning oxidant, the only by-product of the reaction is water, and the post-reaction treatment is easy. At the same time, the price of hydrogen peroxide is rel...

Claims

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Application Information

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IPC IPC(8): C07C45/29B01J31/04B01J31/02
Inventor 曹勇苏杨刘永梅范康年
Owner FUDAN UNIV
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