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Method for preparing acetophenone by oxidizing ethylbenzene in continuous flow micro-channel reactor

A channel reactor, acetophenone technology, applied in the direction of oxidation to prepare carbonyl compounds, etc., can solve the problems of low conversion rate of ethylbenzene, high toxicity, low yield of acetophenone, etc., to improve reaction efficiency, precise temperature control, The effect of increasing selectivity

Inactive Publication Date: 2012-05-02
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has produced a large amount of waste acid, and the pollution to environment is very serious, and catalyst consumption is very large, and the productive rate of acetophenone is generally low
Moreover, benzene is both a reactant and a solvent, and the use of benzene as a solvent is highly toxic.
In addition, metal complexes are often used in industry to prepare acetophenone by oxidation of ethylbenzene under homogeneous high-temperature conditions. This method requires high catalysts, high reaction temperature, and low resource utilization.
JP07196573 discloses the preparation of acetophenone by catalytic oxidation of ethylbenzene with cobalt cycloalkyl carboxylate or cobalt acetate under the action of oxygen, the conversion rate of ethylbenzene is low, and the selectivity of acetophenone is also low
Disclosed in CN101125806A is the method for preparing acetophenone by direct photooxidation of α-methylstyrene under catalyst-free conditions. Low, unable to meet the needs of large-scale industrial production
[0005] So far, there has been no research on the synthesis of acetophenone by liquid-phase catalytic oxidation of ethylbenzene in a microchannel continuous flow mode. The present invention provides a process route for preparing acetophenone by oxidizing ethylbenzene in a continuous flow mode. The process route has the advantages of It lies in the precise control of the reaction temperature, the molar ratio of raw materials and oxidants, and the residence time of the reaction, etc., so that the oxidation product acetophenone can be obtained in a high yield within tens of seconds to several minutes.

Method used

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  • Method for preparing acetophenone by oxidizing ethylbenzene in continuous flow micro-channel reactor
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  • Method for preparing acetophenone by oxidizing ethylbenzene in continuous flow micro-channel reactor

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Embodiment 1

[0027] 1. Raw material preparation: Weigh 34Kg of cobalt acetate, put it into a container with 150L of glacial acetic acid, stir to dissolve it completely, measure 150L of ethylbenzene, pour it into the container, stir, then weigh 16.24KgKBr and add a small amount Water to make it completely dissolved first, pour the completely dissolved KBr solution into the mixed solution, stir evenly, and seal it. Measure 1000L30%H 2 o 2 Put it in another container and seal it.

[0028] 2. In a T-shaped microchannel made of PFA ( image 3 Shown), the channel feature size is 3.14mm. refer to figure 1 Process flow of the present invention utilizes figure 2 The device diagram, according to the following steps: (1) the glacial acetic acid solution of ethylbenzene in the raw material tank 1 enters the microchannel reactor 8 through the pump 3, and the oxidant hydrogen peroxide in the raw material tank 2 enters the microchannel reactor 8 through the pump 4. (2) Continuous flow microchanne...

Embodiment 2

[0031] 1. Raw material preparation: Weigh 15.3Kg of cobalt nitrate, pour it into a container with 300L of acetone, stir to dissolve it completely, measure 150L of ethylbenzene, pour it into the container, stir, then weigh 8.8Kg of NaBr and add A small amount of water to make it completely dissolved first, pour the completely dissolved NaBr solution into the mixed solution, stir evenly, and seal it. Then measure 100mL70%H 2 o 2 Put it in another container and seal it.

[0032] 2. In the coil microchannel made of PFA ( image 3 Shown), the channel feature size is 2.0mm. refer to figure 2 Process flow of the present invention utilizes figure 2 The device diagram, according to the following steps: (1) the glacial acetic acid solution of ethylbenzene in the raw material tank 1 enters the microchannel reactor 8 through the pump 3, and the oxidant hydrogen peroxide in the raw material tank 2 enters the microchannel reactor 8 through the pump 4. (2) Continuous flow microchanne...

Embodiment 3

[0035] 1. Raw material preparation: Weigh 24.5Kg of cobalt acetate, pour it into a 750L container of glacial acetic acid, stir to dissolve it completely, measure 150L of ethylbenzene, pour it into the container, stir, and then weigh 16.38KgKBr Add a small amount of water to make it completely dissolved first, pour the completely dissolved KBr solution into the mixed solution, stir evenly, and seal it. Then measure 1000L80%H 2 o 2 Put it in another container and seal it.

[0036] 2. In the coiled tube microchannel made of stainless steel ( image 3 Shown), the channel feature size is 1.2mm. refer to figure 2 Process flow of the present invention utilizes figure 2 The device diagram, according to the following steps: (1) the glacial acetic acid solution of ethylbenzene in the raw material tank 1 enters the microchannel reactor 8 through the pump 3, and the oxidant hydrogen peroxide in the raw material tank 2 enters the microchannel reactor 8 through the pump 4. (2) Conti...

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Abstract

The invention discloses a method for preparing acetophenone by oxidizing ethylbenzene in a continuous flow micro-channel reactor, which belongs to the technical field of application of organic synthesis, and relates to a novel process for synthesizing acetophenone within the reaction time of dozens of seconds to certain minutes in the continuous flow micro-channel reactor by taking ethylbenzene as a raw material, taking a low-boiling-point common solvent and a cobalt salt as catalysts and taking hydrogen peroxide as an oxidant. Acetophenone serving as a product is obtained lastly by pumping two paths of reaction raw materials into the micro-channel reactor with a metering pump and preheating and reacting. The method is easy and convenient to operate, continuous production of acetophenone at high yield becomes possible, and the process has low environmental pollution. The ethylbenzene transformation ratio is 20-60 percent, and the selectivity of acetophenone is 85-100 percent.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis application, and specifically relates to a method for preparing acetophenone by oxidation of ethylbenzene as a raw material, more specifically, using hydrogen peroxide to oxidize ethylbenzene to prepare acetophenone in a continuous-flow microchannel reactor . Background technique [0002] Acetophenone is an important chemical raw material and an intermediate for the synthesis of other spices. It is mainly used as a solvent, organic synthesis, and olefin polymerization catalyst. Its solubility is similar to that of cyclohexanone. Acetophenone is mainly used as a raw material for pharmaceuticals and other organic synthesis. It is also used to prepare spices, soaps and cigarettes. It can also be used as a solvent for cellulose ethers, cellulose esters and resins, and as a plasticizer for plastics. [0003] At present, the air oxidation method of ethylbenzene is often used in industry to pr...

Claims

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Application Information

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IPC IPC(8): C07C49/78C07C45/28
Inventor 严生虎沈卫张跃沈介发刘建武马兵张沫姜冬明
Owner CHANGZHOU UNIV
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