Method for producing acetophenone through catalytic oxidation of ethylbenzene

A technology for catalytic oxidation and acetophenone, which is applied in the preparation of carbonyl compounds by oxidation, organic chemistry, etc., can solve the problems of difficult separation and recovery of catalysts, inability to recycle and reuse, loss of active components, etc., and achieve easy separation and recycling , Avoid equipment corrosion, strong corrosion resistance effect

Inactive Publication Date: 2012-09-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is a homogeneous catalytic process with a high yield, but the amount of catalyst used is large, the price is expensive, and it cannot be recycled and reused
[0008] From the above, it can be seen that the recovery of supported catalysts is easy to cause the loss of active components, and the homogeneous catalytic oxidation process generally has the disadvantage that the catalyst is difficult to separate and recover.

Method used

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  • Method for producing acetophenone through catalytic oxidation of ethylbenzene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 8.7 g of ethylbenzene and acetonitrile, tert-butyl hydroperoxide and multi-walled carbon nanotubes were added into a closed reaction kettle and mixed to form a mixed suspension. Wherein, the weight ratio of acetonitrile to ethylbenzene is 5.5:1, the weight ratio of multi-walled carbon nanotubes to ethylbenzene is 0.0229:1, and the weight ratio of tert-butyl hydroperoxide to ethylbenzene is 0.03:1. The mixed suspension is heated to 155°C under stirring, and oxygen is introduced to 1.5MPa. Since the reaction process continuously consumes oxygen in a stoichiometric ratio, it is continuously replenished through a pressure stabilizing device and a flow meter connected to an oxygen source during the reaction. Oxygen and keep the pressure constant at 1.5MPa. After reacting for 4 hours, the liquid-solid phase mixture was discharged from the bottom of the reaction kettle, and it was filtered to obtain a solid catalyst and a liquid phase mixture. The liquid phase mixture was anal...

Embodiment 2

[0036] Add 8.7g of ethylbenzene, acetonitrile, and multi-walled carbon nanotubes into a closed reaction kettle and mix to form a mixed suspension. Wherein, the weight ratio of acetonitrile to ethylbenzene is 5.5:1, and the weight ratio of multi-walled carbon nanotubes to ethylbenzene is 0.0229:1. The mixed suspension was heated to 155° C. with stirring, and oxygen was introduced to 1.0 MPa. Oxygen is continuously replenished and kept at a constant pressure of 1.0 MPa through a pressure stabilizing device and a flow meter connected to an oxygen source during the reaction process because oxygen is continuously consumed in a stoichiometric ratio. After reacting for 4 hours, the liquid-solid phase mixture was discharged from the bottom of the reaction kettle, and it was filtered to obtain a solid catalyst and a liquid phase mixture. The liquid phase mixture was analyzed to determine the conversion rate and selectivity of the reaction. The separation and analysis methods of the pr...

Embodiment 3

[0038]8.7 g of ethylbenzene and acetonitrile, phenylethyl hydroperoxide and multi-walled carbon nanotubes were added into a closed reaction kettle and mixed to form a mixed suspension. Among them, the weight ratio of acetonitrile to ethylbenzene is 5.5:1, the weight ratio of multi-walled carbon nanotubes to ethylbenzene is 0.0229:1, and the weight ratio of phenylethyl hydroperoxide to ethylbenzene is 0.03:1. The mixed suspension was heated to 155° C. with stirring, and oxygen was introduced to 2.5 MPa. Oxygen is constantly replenished and kept at a constant pressure of 2.5 MPa through a pressure stabilizing device and a flow meter connected to an oxygen source during the reaction process because oxygen is continuously consumed in a stoichiometric ratio. After reacting for 4 hours, the liquid-solid phase mixture was discharged from the bottom of the reaction kettle, and it was filtered to obtain a solid catalyst and a liquid phase mixture. The liquid phase mixture was analyzed ...

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Abstract

The invention discloses a method for producing acetophenone through catalytic oxidation of ethylbenzene. The method comprises the following steps of: (1) adding the ethylbenzene, a solvent, an initiating agent and a carbon material catalyst into a reactor, and mixing to form mixed suspension liquid; (2) raising the temperature of the mixed suspension liquid obtained in the step (1) to 50-250 DEG C, introducing sufficient oxygen or air which serve as an oxidizing agent, keeping the pressure of 0.1 to 5MPa, and reacting for 0.1 to 20 hours; (3) separating the reaction mixture obtained in the step (2), and thus obtaining a solid catalyst and a liquid phase mixture; and (4) separating the liquid phase mixture obtained in the step (3), and thus obtaining the acetophenone. By the method, the corrosion to equipment and the pollution to the environment due to the usage of acetic acid and a metal catalyst are prevented; the problems that a homogeneous catalyst is difficult to recover and is inactivated in the ethylbenzene oxidation process can be solved; and the method is high in reaction selectivity and high in activity. The catalyst used in the method is high in stability and can be recovered and reused, so that the cost is reduced, and the efficiency is improved.

Description

technical field [0001] The invention relates to a method for preparing acetophenone, in particular to a method for preparing acetophenone in one step through the catalytic oxidation of ethylbenzene, belonging to the technical field of organic synthesis applications. Background technique [0002] Acetophenone is an important organic synthesis intermediate, which is widely used in the synthesis of perfumes, drugs, esters and other organic synthesis raw materials. It is also a good solvent for cellulose ethers, cellulose esters and resins, and a plasticizer for plastics. , has broad application prospects. In the traditional production process of acetophenone, the homogeneous reaction of Friedel-Crafts alkylation is mainly used, that is, it is produced by the reaction of benzene with acetyl chloride, acetic anhydride or acetic acid under the catalysis of stoichiometric anhydrous aluminum trichloride. This method produces a large amount of toxic and corrosive waste liquid, easil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/78C07C45/28
Inventor 彭峰罗金余皓王红娟
Owner SOUTH CHINA UNIV OF TECH
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