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Method for preparing carvone from carveol by heterogeneous catalytic oxidation with molecular oxygen

A technology for catalytic oxidation and carveol, which is applied in the preparation of carbonyl compounds by oxidation, organic chemistry, etc., can solve the problems of difficult separation of catalysts and reactants, high reaction temperature, high catalyst cost, etc., to improve conversion rate and carvone selectivity , reduce the reaction temperature, enhance the effect of economic and environmental benefits

Inactive Publication Date: 2018-05-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction product of this method is more complicated, the product is difficult to purify, and the catalyst cost is higher
Chinese patent CN101613263A discloses a method for preparing carvone by heating and refluxing oxidized carvone oxime with newly prepared or activated manganese dioxide. The method has less pollution, low cost and simple steps, but the product separation needs to be carried out under reduced pressure. higher
The reaction is still a homogeneous reaction in nature, and there is a problem of difficulty in separating the catalyst from the reactant, and the reaction requires a higher reaction temperature and higher energy consumption.

Method used

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  • Method for preparing carvone from carveol by heterogeneous catalytic oxidation with molecular oxygen
  • Method for preparing carvone from carveol by heterogeneous catalytic oxidation with molecular oxygen

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Experimental program
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Effect test

Embodiment 1

[0016] The catalyst used is Rh-W / SiO 2 , the weight composition is Rh%=1.0%, W%=1%, and the rest is carrier SiO 2 . The preparation steps of the catalyst specifically include: a) using the required amount of rhodium chloride and ammonium metatungstate to prepare a mixed aqueous solution; b) impregnating the silica gel carrier with a required particle size of 20-40 meshes; c) obtaining the above-mentioned equal-volume impregnation The solid was dried at 100°C for 3 hours; d) After drying, the carrier was calcined at 450°C for 3 hours to obtain Rh-W / SiO 2 catalyst. The evaluation of the catalytic performance of the catalyst on the oxidation of carveol to carvone is carried out on a fixed bed reactor, the catalyst loading is 2.0g, the raw material is a xylene solution containing carveol with a weight content of 16.7%, and the reaction temperature is 110°C , the reaction pressure is normal pressure, and the liquid space velocity is 0.2h -1 , molecular oxygen is oxygen, and its...

Embodiment 2

[0018] The liquid space velocity of carvone solution is 0.65h -1 , other conditions are identical with embodiment 1.

Embodiment 3

[0020] The liquid space velocity of carvone solution is 1.2h -1 , other conditions are identical with embodiment 1.

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Abstract

The invention relates to a method for preparing carvone from carveol by heterogeneous catalytic oxidation with molecular oxygen. A reaction system comprises carveol, a solvent, molecular oxygen and asolid catalyst; the reaction temperature is 50-200 DEG C, reaction pressure is normal pressure-1.0 MPa, the weight content of carveol in a reaction substrate is 10%-40%, liquid space velocity of the carveol solution is 0.2 h<-1>-2.0 h<-1>, and the gas space velocity is 1000 h<-1>-3000 h<-1>. The solid catalyst uses silica gel as a carrier and comprises one of noble metals such as Rh, Pd, Pt and Ru, and contained aids are one or more than two of W, Mo, Ce, La, Fe, Co, Ti, and Zr; under mild reaction conditions, carveol can be efficiently converted into carvone under the action of the solid catalyst. Catalytic activity and carvone selectivity of the solid catalyst remain basically unchanged in the 1000-hour stability test.

Description

technical field [0001] The invention relates to a reaction process and catalyst for one-step preparation of carvone by catalytic oxidation of carveol molecular oxygen under the action of a supported noble metal catalyst. Background technique [0002] The scientific name of carvone is 1-methyl-4-isopropen-6-cyclohexen-2-one, which is one of the main components of many plant essential oils, and is also the main component of the deployment of high-grade food flavors and high-grade cosmetics flavors , widely used in daily life. Carvone is also a natural antioxidant, has good antioxidant activity, and can also be used as a high-efficiency solvent in industry. Carvone has now become a bulk spice, and the demand is increasing year by year. [0003] At present, there are mainly two types of sources of carvone, natural and synthetic. Carvone extracted from natural essential oils has the disadvantages of low output and high price, and is limited by natural conditions and seasons, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/29C07C49/647
CPCC07C45/29C07C49/647
Inventor 龚磊峰丁云杰宋宪根
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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