Method for preparing cyclohexanone by cyclohexane oxidation

A technology of cyclohexanone and cyclohexane, applied in the field of preparation of cyclohexanone, can solve the problems of low two-phase mass transfer efficiency, many by-products, etc. Effect

Pending Publication Date: 2022-02-25
CHINA PETROLEUM & CHEM CORP +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention provides a method for preparing cyclohexanone by oxidation of cyclohexane to solve the problems of low efficiency of two-phase mass transfer and many by-products caused by back-mixing in the existing series reaction of still-type cyclohexanone oxidation by cyclohexane

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  • Method for preparing cyclohexanone by cyclohexane oxidation

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preparation example Construction

[0024] see figure 1 , the present invention provides a technical solution, a method for producing cyclohexanone by oxidation of cyclohexane, comprising a device for producing cyclohexanone by oxidation of cyclohexane, and the device for producing cyclohexanone by oxidation of cyclohexane includes a tubular reactor 1. Ultrasonic microbubble generator 2, air storage tank 3, cyclohexane storage tank 4, condenser 5 and gas-liquid separator 6, characterized in that the preparation method comprises the following steps:

[0025] Step 1: The air storage tank 3 and the cyclohexane storage tank 4 are fed in a certain proportion, and the mixing is strengthened by the ultrasonic microbubble generator 2, so that the gas is broken into microbubbles and enters the tubular reactor 1. After the reaction, the materials pass through the condenser 5 cooling, gas-liquid separator 6 separation to obtain cyclohexane oxidation liquid;

[0026] Step 2: catalytically decompose the cyclohexane oxidatio...

Embodiment 1

[0028] The spiral dividing plate (102) in the tubular reactor (1) forms an included angle of 45° with the reactor axis, and the reaction temperature in the tubular reactor (1) is controlled by the heat exchange tube (103) to be 130°C. The pressure is 1.5MPa, the air feed rate is controlled to make the reaction gas-liquid separation, and the oxygen volume content in the gas phase is 1.2%, and the diameter of the microbubbles entering the tubular reactor (1) is 0.3mm. The chromium ion concentration of the ester catalyst is 8ppm, and under the conditions of a reaction temperature of 100°C, it decomposes slightly acidicly for 30 minutes, and then decomposes alkalinely for 20 minutes.

[0029] Cyclohexane oxidation per pass conversion rate 7.9%, selectivity of cyclohexanol, cyclohexanone and cyclohexyl hydroperoxide 93%, decomposition rate of cyclohexyl hydroperoxide 99.8%, total yield of cyclohexanone and cyclohexanol 99.5% , The ratio of ketone to alcohol is 1.4:1.

Embodiment 2

[0031] The spiral partition plate 102 in the tubular reactor 1 forms an included angle of 75° with the reactor axis, and the reaction temperature in the tubular reactor 1 is controlled by the heat exchange tube 103 to be 160°C, the reaction pressure is 0.5MPa, and the air inlet is controlled. The volume content of oxygen in the gas phase is 1.0% after the reaction gas-liquid separation, the diameter of the microbubbles entering the tubular reactor 1 is 0.1mm, and the chromium ion concentration of the oil-soluble isooctyl chromate catalyst is 2ppm, and the reaction temperature Under the condition of 130°C, first decompose slightly acidic for 60 minutes, and then decompose alkalinely for 60 minutes.

[0032] Cyclohexane oxidation per pass conversion rate 7.3%, selectivity of cyclohexanol, cyclohexanone and cyclohexyl hydroperoxide 95%, decomposition rate of cyclohexyl hydroperoxide 99.7%, total yield of cyclohexanone and cyclohexanol 99.5% , The ratio of ketone to alcohol is 1.3...

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Abstract

The invention discloses a method for preparing cyclohexanone by cyclohexane oxidation. The method involves a device for preparing cyclohexanone by cyclohexane oxidation, and the device for preparing cyclohexanone by cyclohexane oxidation comprises a tubular reactor, an ultrasonic microbubble generator, an air storage tank, a cyclohexane storage tank, a condenser and a gas-liquid separator. The preparation method comprises the following steps: 1, feeding materials into the air storage tank and the cyclohexane storage tank according to a certain proportion, intensively mixing through the ultrasonic microbubble generator to crush gas into microbubbles, feeding the microbubbles into the tubular reactor, cooling the reacted materials through the condenser, and separating through the gas-liquid separator to obtain a cyclohexane oxidation liquid; and 2, carrying out catalytic decomposition on the cyclohexane oxidation liquid obtained in the step 1 under a slightly acidic condition to obtain cyclohexanol and cyclohexanone, and carrying out extractive distillation separation to obtain cyclohexanone. The conversion per pass of cyclohexane and the yield of cyclohexanone are high, and the material consumption and the energy consumption are obviously reduced.

Description

technical field [0001] The invention relates to the technical field of preparation of cyclohexanone, in particular to a method for preparing cyclohexanone by oxidation of cyclohexane. Background technique [0002] Cyclohexanone is an important basic chemical raw material, mainly used to produce caprolactam and adipic acid, etc., and caprolactam is further processed to produce nylon fiber or engineering plastics. Cyclohexanone production at home and abroad mainly adopts cyclohexane oxidation method and cyclohexene hydration method. At present, the oxidation section of the cyclohexane oxidation process adopts a traditional multi-pot series reactor, and the air is bubbled into cyclohexane through the small holes of the distributor. The bubble size is 3-30mm, the specific surface area is 200-500m2 / m3, and the mass transfer performance Poor, single-pass conversion rate of cyclohexane oxidation is 3-4%, selectivity ≤ 85%, many side reactions, low single-pass conversion rate, resu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/33C07C49/603
CPCC07C45/33C07C49/603
Inventor 杨忠林华兵赵思远金汉强季峰崎任磊孔伟伟张蓉蓉金钢
Owner CHINA PETROLEUM & CHEM CORP
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