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Method for preparing cyclohexanone with cyclohexane liquid-phase oxidation process

A liquid phase oxidation method, cyclohexane technology, applied in the separation/purification of carbonyl compounds, organic chemistry and other directions, can solve the problems affecting the quality of the product cyclohexanone, achieve better separation effect, less fixed investment and stable operation Effect

Inactive Publication Date: 2016-05-25
QUZHOU JUHUA POLYAMIDE FIBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The analysis found that after oxidative decomposition and water washing of cyclohexane oxidation liquid, after rectification and removal of alkanes, the content of cyclohexyl hydroperoxide in the rectification tower still was between 0.05% and 0.1%. During the operation of separating cyclohexanone, it will continue to decompose and produce impurities, so that the content of hexanal in the cyclohexanone product will still be tens of ppm, and it will also contain a small amount of ester, thus affecting the quality of the product cyclohexanone
In addition, the original by-products such as heteroketones and aldehydes are also difficult to separate during the rectification process, which ultimately further affects the quality of the product cyclohexanone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The alcohol and ketone mixed solution containing alkane 50wt% that the three-effect alkane tower rectification operation obtains is in 40m 3 / h enters the feed heater 1 for heating, and after heating to 94.5°C, the flow rate is 0.3m 3 / h fresh sodium hydroxide solution enters the first static mixer 2 together, and then enters the first saponification tower 4 (Φ800×15000, Pall ring packing, operating temperature is 91.0°C) from the bottom, and the second saponification tower 5 (Φ800×15000, Pall ring packing, operating temperature is 90.0°C), relying on pressure difference to overflow from the top of the second saponification tower 5 and enter the first separator 6 (horizontal tank separator, Φ3200×7000, V= 65.5m 3 ). The first separator 6 (Φ3200×7000, V=65.5m 3 ) bottom lye, through circulation pump 3, most (8m 3 / h) circulating to the first static mixer 2, a small portion (1.2m 3 / h) to control the first separator 6 (Φ3200×7000, V=65.5m 3 ) Alkaline oil interface,...

Embodiment 2

[0032] The alcohol and ketone mixed solution containing alkane 55wt% that the three-effect alkane tower rectification operation obtains is in 42m 3 / h into the feed heater 1 for heating, after heating to 93.5°C, the flow rate is 0.28m 3 / h of fresh sodium hydroxide solution enters the first static mixer 2 together, and then enters the first saponification tower 4 (Φ800×15000, Pall ring packing, operating temperature is 93.8 ° C) from the bottom, and the second saponification tower 5 (Φ800×15000, Pall ring packing, operating temperature is 93°C), relying on pressure difference to overflow from the top of the second saponification tower 5 and enter the first separator 6 (Φ3200×7000, V=65.5m 3 ). The first separator 6 (Φ3200×7000, V=65.5m 3 ) bottom lye, through circulation pump 3, most (8.2m 3 / h) circulating to the first static mixer 2, a small portion (1.0m 3 / h) to control the first separator 6 (Φ3200×7000, V=65.5m 3 ) Alkaline oil interface, sent to the previous process....

Embodiment 3

[0034] The alcohol and ketone mixed solution containing alkane 53wt% that the three-effect alkane tower rectification operation obtains is in 39m 3 / h enters the feed heater 1 for heating, and after heating to 93.0°C, the flow rate is 0.25m 3 / h of fresh sodium hydroxide solution enters the first static mixer 2 together, and then enters the first saponification tower 4 (Φ800×15000, Pall ring packing, operating temperature is 93.4 ° C) from the bottom, and the second saponification tower 5 (Φ800×15000, Pall ring packing, operating temperature is 92.5°C), relying on pressure difference to overflow from the top of the second saponification tower 5 and enter the first separator 6 (Φ3200×7000, V=65.5m 3 ). The first separator 6 (Φ3200×7000, V=65.5m 3 ) bottom lye, through circulation pump 3, most (7.9m 3 / h) circulating to the first static mixer 2, a small portion (0.9m 3 / h) to control the first separator 6 (Φ3200×7000, V=65.5m 3 ) Alkaline oil interface, sent to the previous...

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Abstract

The invention discloses a method for preparing cyclohexanone with a cyclohexane liquid-phase oxidation process. The method comprises processes including cyclohexane oxidation reaction solution synthesis, oxidation solution decomposition and washing, triple-effect alkane tower rectification, alkane four-tower rectification, twice saponification, coarse alcohol ketone continuous rectification and obtaining of cyclohexanone. The method is characterized in that the sequence of the processes is cyclohexane oxidation reaction solution synthesis, oxidation solution decomposition and washing, triple-effect alkane tower rectification, twice saponification, alkane four-tower rectification and coarse alcohol ketone continuous rectification to obtain cyclohexanone. The method can fully decompose cyclohexyl hydroperoxide, substantially reduce impurities such as aldehyde, ester and miscellaneous ketone in cyclohexanone, and improve the quality of cyclohexanone. The method has the advantages of simple process, low investment and cost, good separation effect and apparent impurity removal.

Description

technical field [0001] The invention belongs to the field of new petrochemical materials, and in particular relates to a method for preparing cyclohexanone by a cyclohexane liquid-phase oxidation method. Background technique [0002] Cyclohexanone is an important organic chemical product, an important organic chemical raw material, and the main intermediate for the preparation of caprolactam and adipic acid. The industrial production processes of cyclohexanone in the world mainly include phenol hydrogenation method, cyclohexane liquid phase oxidation method, and cyclohexene hydration method. Among them, the cyclohexane liquid-phase oxidation method is currently the main method for the industrial production of cyclohexanone due to its mature process, abundant sources of benzene as a starting material, and good product quality. [0003] The existing cyclohexane liquid-phase oxidation method for preparing cyclohexanone production process includes synthesizing cyclohexane oxida...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/78C07C45/85C07C45/82C07C45/80C07C49/403
CPCC07C45/78C07C45/80C07C45/82C07C45/85C07C49/403
Inventor 夏碧波朱海峰谷灿波贺辉龙吴平华曹彬
Owner QUZHOU JUHUA POLYAMIDE FIBER
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