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Cogeneration method of methyl isobutyl ketone and diiso butyl ketone

A technology of methyl isobutyl ketone and diisobutyl ketone, applied in the field of preparation of pharmaceutical intermediates, can solve the problems of no industrial production, unsatisfactory, low diisobutyl ketone selectivity, etc., and achieves increased risk resistance Capability, cost of use reduction, high product yield effect

Active Publication Date: 2014-04-30
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Diisobutyl ketone (DIBK) is a by-product of the process of preparing methyl isobutyl ketone in industry, but the selectivity of diisobutyl ketone produced in this process is very low, accounting for only 0.2~ of the amount of methyl isobutyl ketone 0.3%, has been unable to meet the increasing demand of the current market; there are other reports to generate porone by acid-catalyzed condensation of acetone, and hydrogen reduction to diisobutyl ketone and preparation method, but there is no report of industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The catalyst of Zhejiang Xinhua Chemical Co., Ltd.'s own brand XH-A-69 is installed in the reactor, and its composition and mass content are as follows: the content of copper is 0.5-15%, the content of palladium is 0.05-0.1%, and the content of zirconium is 0.1-1.5%, the zinc content is 0.3-5%, and the alumina is γ-alumina.

[0037] The reaction temperature is 145°C, the reaction pressure is 0.5MPa, the liquid space velocity of isopropanol is 0.5L isopropanol / (L catalyst·hour), and the molar ratio of acetone:isopropanol is 1:1. Reaction result: the conversion rate of isopropanol is 53%, the selectivity of methyl isobutyl ketone is 65%, and the selectivity of diisobutyl ketone is about 33%. Wherein the mixed solution separation process after the reaction is specifically as follows:

[0038] (1) Separation of unreacted acetone from the reaction mixture:

[0039] The reaction mixture enters the light removal tower, and after rectification and separation, the unreacted ac...

Embodiment 2

[0047] Use catalyst in the reactor with embodiment 1.

[0048] The reaction temperature is 170°C, the reaction pressure is 1.8MPa, the liquid space velocity of isopropanol is 1.2L isopropanol / (L catalyst·hour), and the molar ratio of acetone:isopropanol is 2:1. Reaction result: the conversion rate of isopropanol is 70%, the selectivity of methyl isobutyl ketone is 70%, and the selectivity of diisobutyl ketone is about 26%. The separation process of the mixed solution after the reaction is specifically the same as in Example 1.

Embodiment 3

[0050] The composition and mass content of the catalyst used in the reactor are as follows: copper content is 3%, palladium content is 0.05%, zirconium content is 1.0%, zinc content is 2.3%, alumina is γ-alumina, which is modified by magnesium oxide Alumina with 5% magnesia in an alumina support.

[0051] The reaction temperature is 150°C, the reaction pressure is 1.5MPa, the liquid space velocity of isopropanol is 1.0L isopropanol / (L catalyst·hour), and the molar ratio of acetone:isopropanol is 4:1. Reaction result: the conversion rate of isopropanol is 82%, the selectivity of methyl isobutyl ketone is 78%, and the selectivity of diisobutyl ketone is about 19%. The separation process of the mixed solution after the reaction is specifically the same as in Example 1.

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Abstract

The invention relates to a preparation method of a medical intermediate, and particularly relates to a cogeneration method of methyl isobutyl ketone and diiso butyl ketone. The method comprises the following steps: mixing and preheating acetone and isopropanol, entering a reactor containing copper-palladium-zirconium-zinc / molybdenum oxide catalysts; generating a reaction mixed solution of taking methyl isobutyl ketone and diiso butyl ketone as main ingredients from the acetone in a manner of reaction under the conditions that the reaction temperature is 130-210 DEG C, the reaction pressure is 0.1-4.0MPa, the liquid phase airspeed of isopropanol is 0.1-2.5h<-1> and the ketone alcohol mole ratio is 1-7; separating and refining, so as to obtain the methyl isobutyl ketone product and the diiso butyl ketone product. The cogeneration method has the advantages that the use cost of the catalyst is greatly reduced, and the method is low in energy consumption, simple in equipment, free of special requirements, fewer in heavy constituents, high in acetone utilization rate and high in product yield.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, in particular to a method for the joint production of methyl isobutyl ketone and diisobutyl ketone. Background technique [0002] Methyl isobutyl ketone (MIBK) is a colorless, transparent medium-boiling point ketone solvent and chemical intermediate with excellent performance and an aromatic ketone odor. Miscible with most organic solvents, it can be used as paint, nitrocellulose, ethyl cellulose, audio and video tape, paraffin and various natural or synthetic resin solvents, dewaxing agent for lubricating oil refining, rare earth metal extraction agent, polymer reaction initiator Agents, surfactants, pharmaceuticals, pesticide extractants and raw materials for rubber antioxidants, etc. It is a fine petrochemical intermediate that is currently in short supply in my country. It is irreplaceable in many application fields. The current demand mainly depends on imports. [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/04C07C45/71C07C45/78
CPCC07C45/71C07C45/78C07C49/04
Inventor 兰昭洪包江峰王卫明徐利红王晓明段小刚王东岳邵建强吴锦平
Owner ZHEJIANG XINHUA CHEM
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