Method for catalyzing cyclone oxide to synthesizing lactone by using nano magnesium-base catalyst

A technology using magnesium-based catalysts and catalytic oxidation, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of small reaction TON, low repeatability, low catalytic efficiency, etc., to achieve Low cost, high catalytic activity and high selectivity

Inactive Publication Date: 2008-05-28
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this catalyst system has not been used in the research of synthesizing other lactones, and the reproducibility is not high. Although the conversion rate and selectivity of the oxidation reaction of cyclohexanone BV can reach 100%, the reaction TON is small and the catalytic efficiency is low. Low
In addition, due to the lack of relevant research, the author did not try the influence of other Mg-based compounds on the reaction, especially the influence of catalyst morphology on catalytic activity has not been reported.

Method used

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  • Method for catalyzing cyclone oxide to synthesizing lactone by using nano magnesium-base catalyst

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Experimental program
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Effect test

Embodiment 1

[0016] Embodiment 1: the preparation of sheet-like Mg-based catalyst: 0.02mol MgCl 2 ·6H 2 O and 0.02mol CO(NH 2 ) 2 dissolved in 10mL H 2 O, stirred at 30°C to obtain a clear solution, and added dropwise a volume fraction of 2.5% NH 3 ·H 2 O adjusts pH=8. Stirring was continued for 2 h, and the resulting white suspension was placed in a 200 mL hydrothermal kettle, crystallized at 323 K for 2 h, and suction filtered. The obtained product was washed successively with distilled water and ethanol, dried, and calcined at 373K for 2 hours in an air atmosphere to obtain the catalyst. The reaction conditions adopted are: 0.0029mol cyclohexanone, 2.4mL molar ratio is 1: 0.5 mixed solution of benzonitrile and 1,4-dioxane, 0.9mL of 10% H 2 o 2 , control bath temperature 303K, react for 2 hours, the consumption of catalyst is 0.2 of the mole number of raw material cyclohexanone. Record it as 1#. After the reaction is completed, the analysis results are shown in Table 1.

Embodiment 2

[0017] Embodiment 2: the preparation of flake Mg-based catalyst: 0.04mol MgCl 2 ·6H 2 O and 0.04mol CO(NH 2 ) 2 dissolved in 20mL H 2 O, stirred at 40°C to obtain a clear solution, and added dropwise a volume fraction of 2.5% NH 3 ·H 2 O adjusts pH=9. Stirring was continued for 4 h, and the resulting white suspension was placed in a 200 mL hydrothermal kettle, crystallized at 373 K for 4 h, and suction filtered. The obtained product was washed successively with distilled water and ethanol, dried, and calcined at 473K for 4 hours in an air atmosphere to obtain the catalyst. The reaction conditions adopted are: 0.0029mol cyclohexanone, 2.4mL molar ratio is 1: 1.0 mixed solution of benzonitrile and 1,4-dioxane, 1.2mL of 20%H 2 o 2 , control bath temperature 313K, react for 4 hours, the consumption of catalyst is 0.3 of the mole number of raw material cyclohexanone. Record it as 2#. After the reaction is completed, the analysis results are shown in Table 1.

Embodiment 3

[0018] Embodiment 3: the preparation of sheet-like Mg-based catalyst: 0.08mol MgCl 2 ·6H 2 O and 0.08mol CO(NH 2 ) 2 Dissolve in 30mL H 2 O, stirred at 50°C to obtain a clear solution, and added dropwise a volume fraction of 2.5% NH 3 ·H 2 O adjusts pH=10. Stirring was continued for 6 h, and the resulting white suspension was placed in a 200 mL hydrothermal kettle, crystallized at 423K for 6 h, and suction filtered. The obtained product was washed successively with distilled water and ethanol, dried, and calcined at 573K for 6 hours in an air atmosphere to obtain the catalyst. The reaction conditions adopted are: 0.0029mol cyclohexanone, 2.4mL molar ratio is 1: 1.5 mixed solution of benzonitrile and 1,4-dioxane, 1.5mL of 30%H 2 o 2 , control bath temperature 323K, react for 6 hours, the consumption of catalyst is 0.4 of the mole number of raw material cyclohexanone, denoted as 3#. After the reaction is completed, the analysis results are shown in Table 1.

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Abstract

The invention relates to chemical technical field, in particular to a method for using magnesia catalyst to catalyze and oxidize cyclone to synthesize lactone. The invention uses some nanometer sheet magnesia compound as catalyst, uses mixture of cyanobenzene and 1, 4-dioxane at a certain proportion as solvent, at a special reaction temperature, to catalyze and oxidize cyclone to synthesize lactone compound. The invention uses commercial cyclopentanone, cyclohexanone and adamantaneketone as raw materials, at mild condition, to reach the total yield of lactone compound more than 90%. The invention uses hydrogen dioxide water solution as oxidant, to eliminate the environment pollution of traditional oxidation process as peroxyacid, to realize environment-friend catalysis conversion. The invention has low cost, which can be used for industrialized lactone compound production.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for synthesizing lactone compounds by catalytically oxidizing cyclic ketones with a nano-magnesium-based catalyst. Background technique [0002] The Baeyer-Villiger (BV) oxidation reaction is an important class of reactions that oxidize cyclic ketones or chain ketones into lactones or esters. In view of the fact that this reaction can control the stereostructure of the product, the conversion of functional groups and ring formation in organic synthesis Expansion matters. The oxidant used in the traditional BV oxidation reaction is generally a peroxyacid (such as trifluoroperoxyacetic acid, peroxybenzoic acid, m-chloroperoxybenzoic acid, etc.). The oxidants used are all chemical oxidants. These oxidants have some general disadvantages, such as serious environmental pollution, large acid pollution, large amount of three wastes, difficult separation a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D313/04C07D309/30C07D313/10B01J21/10B01J27/236
Inventor 戴维林李静霞范康年
Owner FUDAN UNIV
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