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A kind of preparation method of methyl ethyl ketone

A technology of methyl ethyl ketone and n-butane, which is applied in the field of organic compound preparation, can solve the problems of low conversion rate and selectivity of methyl ethyl ketone, achieve the effects of avoiding the problem of explosion limit, less catalyst consumption, and mild reaction conditions

Active Publication Date: 2022-05-03
SUN YAT SEN UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention aims at the problem of low conversion rate and selectivity of methyl ethyl ketone prepared by catalyzing n-butane when air is used as an oxidant in the prior art, and provides a method for preparing methyl ethyl ketone. The preparation method can use air as an oxidant to effectively catalyze n-butane Butane is prepared to obtain methyl ethyl ketone, wherein the conversion rate of n-butane is greater than 10%, and the selectivity of methyl ethyl ketone is not less than 55%

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  • A kind of preparation method of methyl ethyl ketone
  • A kind of preparation method of methyl ethyl ketone
  • A kind of preparation method of methyl ethyl ketone

Examples

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preparation example Construction

[0025] The synthetic method of the binuclear copper porphyrin catalyst used in the present invention, step is as follows:

[0026] Under the condition of room temperature and argon protection, the [26] six-membered porphyrin corresponding to the halogen, anhydrous copper acetate, anhydrous sodium acetate, and dichloromethane are sequentially added into the reaction bottle, and reacted for 3 to 10 hours. The reaction liquid that has reacted is extracted with distilled water, collects organic layer, uses silica gel column chromatography, obtains black solid powder, obtains binuclear copper porphyrin, and its structure is shown in general formula (I):

[0027]

[0028] Wherein M is Cu, and R is selected from halogen.

[0029] The metalloporphyrin catalyst used in the comparative example was also prepared by the above-mentioned similar preparation method.

Embodiment 1

[0031] In the autoclave, add the 1,2-dichloroethane containing the binuclear copper porphyrin (M=Cu, R=Cl) of the general formula (I) structure as the catalyst, add the free radical initiator NHPI, and fill the normal Butane and 1MPa air were reacted at 60° C. for 8 hours; the amount of catalyst used was 0.003% of the molar weight of n-butane, and the amount of free radical initiator was 1.5% of the molar weight of n-butane.

Embodiment 2～18 and comparative example 1～4

[0033] The catalytic methods and reaction conditions of Examples 2 to 18 and Comparative Examples 1 to 4 are basically the same as in Example 1, the differences are shown in the following table 1, wherein A represents that the catalyst consumption is the molar percentage of n-butane, and B represents free Base initiator consumption is the mole percentage of n-butane:

[0034] Table 1

[0035]

[0036]

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Abstract

The invention provides a method for preparing methyl ethyl ketone. The preparation method uses n-butane as a raw material, disperses n-butane, a free radical initiator and a catalyst in a solvent, uses air as an oxidant, and reacts at a reaction temperature of 50 to 90 ℃, reaction pressure is 0.5~1.5MPa under the condition of reaction 6~10h, catalytic oxidation n-butane is obtained methyl ethyl ketone; The catalyst is the binuclear copper porphyrin compound of following general formula (I) structure, wherein M is Cu, R All are selected from halogen; the dosage of the catalyst is 0.0001-0.005% of the molar weight of n-butane, and the dosage of the free radical initiator is 1-2% of the molar weight of n-butane. The preparation method of the present invention can use air as an oxidant to directly oxidize n-butane to prepare methyl ethyl ketone in a one-step method. The reaction conditions are mild and the amount of catalyst is small, which effectively avoids the problem of the explosion limit of n-butane and ensures the single-pass of butane at the same time. The conversion rate and selectivity meet the needs of industrial production applications.

Description

technical field [0001] The present invention relates to the technical field of organic compound preparation, more specifically, to a kind of preparation method of methyl ethyl ketone. Background technique [0002] Methyl ethyl ketone, also known as 2-butanone or methyl ethyl ketone, is a colorless transparent liquid at room temperature with a smell similar to acetone. It is an organic solvent with excellent performance and wide uses. It is also used for the preparation of medicines, dyes, detergents, Spices, antioxidants and intermediates of some catalysts, also used as a developer after photolithography of integrated circuits. [0003] The source of n-butane is abundant, cheap and easy to get, so the process of preparing methyl ethyl ketone with higher added value by direct oxidation of n-butane with oxygen or air as oxidant has attracted much attention. In most of the currently disclosed methods for preparing methyl ethyl ketone by n-butane oxidation, either the selectivi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/33C07C49/10B01J31/18
CPCC07C45/33B01J31/183B01J2531/16B01J2531/025B01J2231/70C07C49/10
Inventor 纪红兵陈虹宇徐圣周贤太
Owner SUN YAT SEN UNIV