Bifunctional catalyst for preparing 3-pentanone through methanol-butanone alkylation and preparation method and application thereof

Abstract

The invention relates to the field of organic synthesis catalysis, and discloses a bifunctional catalyst for preparing 3-pentanone through methanol-butanone alkylation and a preparation method and application thereof. The bifunctional catalyst is prepared from the following components in percentage by mass: 2.0 to 30 percent of nickel oxide, 40 to 90 percent of magnesium oxide, 10 to 30 percent ofaluminum oxide and 0 to 20 percent of zinc oxide. The catalyst is used in a reaction for producing 3-pentanone through gas-solid phase methanol-butanone alkylation, and the bifunctional catalyst hasgood 3-pentanone selectivity and stability, and can realize the reaction at a low temperature. In the reaction, the reaction temperature is controlled to be 220-350 DEG C at the normal pressure, and the mass ratio of methanol to butanone in the raw materials is (5-15): 1; and the contact time of the reaction materials and the catalyst is controlled to be 0.5-25 ml / g of the catalyst / h, and high-yield 3-pentanone 60-70% can be obtained.

Description

technical field [0001] The invention relates to the field, in particular to a bifunctional catalyst for preparing 3-pentanone by alkylation of methanol-butanone, a preparation method and application thereof. Background technique [0002] 3-pentanone, also known as 1,3-dimethylacetone, diethyl (base) ketone, diethyl ketone, diethyl ketone, etc., the molecular formula is CH 3 CH 2 COCH 2 CH 3 , CAS No. 96-22-0, is a colorless liquid with acetone odor. 3-Pentanone is often used as a solvent, as well as a drug intermediate, chemical reagent and organic synthesis raw material; it can be used to synthesize the herbicide pendimethalin, etc. [0003] At present, 3-pentanone is mainly prepared by 3-pentanol oxidation method, which needs to be oxidized with sodium dichromate oxidant in the presence of concentrated sulfuric acid, and the reaction temperature is about 90°C. After the reaction is completed, first filter and separate the generated solid waste and catalyst, and then c...

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Problems solved by technology

However, there is no special literature report at present, and it is a new synthetic process

[0005] In published patents and documents, typical ketone alkylation catalytic synthesis technology has the methyl ethyl ketone (MEK) method of Japanese patent P2000-26360A, adopts the liquid-phase catalytic reaction process, with methyl ethyl ketone and 35% formaldehyde aqueous solution is used as raw material, in 10% NaOH aqueous solution, Pd / C is catalyst, the temperature is 60 ℃, under the hydrogen pressure of about 0.40~0.45MPa, catalytic hydrogenation synthesis methyl isopropyl ketone, formaldehyde The yield of methyl isopropyl ketone is 73%; Although a small amount of 3-pentanone is also generated in this process, the amount of reaction waste liquid is large and the catalyst is expensive

In recent years, in order to facilitate continuous production, gas-solid phase methyl isopropyl ketone (MIPK) synthesis technology has attracted the attention of many people; this process uses methanol to replace formaldehyde and directly reacts with methyl ethyl ketone, and there is a certain cost in raw material cost. advantages; however, so far, the target and main product of this process is still methyl isopropyl ketone

The patent EP0224218 of the German BASF company discloses a catalyst made of composite oxides containing Ce, Cr, Fe, Mg, Mn, etc., but there are problems such as high reaction temperature (500°C) and easy coking on the surface of the catalyst.

Chinese patent CN1733360A describes a catalyst made of a mixed oxide of Zr, Mn, Zn and alkali metals loaded with a small amount of Pd noble metal. Although the reaction temperature is lower than 400 ° C, the surface of the catalyst is slightly coked, but there are catalysts containing noble metals The disadvantages of high price, poor catalyst stability and low utilization rate of raw material methanol limit the application of large-scale industrial production

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