A kind of liquid phase oxidation method of cyclohexane

A cyclohexane and said technology are applied in chemical instruments and methods, hydrocarbon oxidation to prepare oxygen-containing compounds, organic chemistry, etc., and can solve the problems of large cyclohexane circulation, high energy consumption, cyclohexanone and cyclohexanol Low yield and other problems, to achieve the effect of improving reaction rate and heat transfer rate, strong heat transfer efficiency, and safety assurance

Active Publication Date: 2011-11-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In short, due to the current production process, there are large cyclohexane circulation, high energy consumption, low yields of cyclohexanone and cyclohexanol, large environmental pollution, low safety, long reaction time, and low reactor efficiency.

Method used

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  • A kind of liquid phase oxidation method of cyclohexane
  • A kind of liquid phase oxidation method of cyclohexane
  • A kind of liquid phase oxidation method of cyclohexane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] It adopts the form of micro-channel reactor, see the structure of liquid inlet and micro-channel figure 1 , The size of the reaction microchannel is the same as the inlet size.

[0061] Reaction process see image 3 . The microchannel reactor disc is 5cm wide, 6cm long, and 2mm thick; the channels are divided into four groups, each group has five channels, the channel length is 50mm, and the spacing is 0.5mm; the spacing of each group is 2mm, and there is a 2mm lower part of each sub-channel entrance 1 micropore of 200μm×200μm; correspondingly designed on the back of the reaction disk corresponding to short channels, gas-liquid T-type mixing, square channel with gas inlet channel size of 300μm×300μm, gas inlet and liquid inlet are perpendicular; liquid inlet size is 300μm×300μm square channel.

[0062] The cyclohexane oxidation reaction is carried out with pure oxygen as the oxidant. The initiator in the cyclohexane solution is a mixture of cyclohexanone and cyclohexanol wi...

Embodiment 2

[0064] Reaction process see image 3 . The reactor is a micro-coiled tube reactor with an inner diameter of 0.53mm and a length of 50m. Air is used as the oxidant for the cyclohexane oxidation reaction. The initiator in the cyclohexane solution is a mixture of cyclohexanone and cyclohexanol with a mass ratio of 1:1, accounting for 0.5% of the weight of cyclohexane. The reaction temperature is 170°C and the pressure 1.3MPa, residence time 5min, gas / liquid molar ratio 1.0:1. The conversion rate of cyclohexane is 2.5%, and the total selectivity of cyclohexanone, cyclohexanol, and cyclohexyl hydroperoxide is 98%.

Embodiment 3

[0066] Reaction process see image 3 . The reactor is a micro-coiled tube reactor with an inner diameter of 1.3mm and a length of 12m. Air is used as the oxidant to carry out the cyclohexane oxidation reaction. The initiator in the cyclohexane solution is a mixture of cyclohexanone and cyclohexanol with a mass ratio of 1:1, accounting for 0.8% of the weight of cyclohexane. The reaction temperature is 165°C and the pressure 1.25MPa, residence time 5min, gas / liquid molar ratio 1.1:1. The conversion rate of cyclohexane is 3.5%, and the total selectivity of cyclohexanone, cyclohexanol, and cyclohexyl hydroperoxide is 86%.

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Abstract

A liquid-phase oxidation method of cyclohexane, characterized in that the method is a reaction at a temperature of 145-200°C, a pressure of 0.8-2.5MPa, and a molar ratio of molecular oxygen-containing gas to cyclohexane of 0.1-10:1 The method is carried out in a microreactor under certain conditions, and the residence time of the reaction material is 0.5-30min. The said microreactor is a microchannel reactor and / or a microtube reactor. The method has safety, strengthens the transfer of heat, can significantly increase the reaction speed of cyclohexane oxidation, and improves the total selectivity of cyclohexanone, cyclohexanol and cyclohexyl hydroperoxide.

Description

Technical field [0001] The invention relates to a liquid phase oxidation method of cyclohexane, and more specifically to a method for preparing cyclohexanone and cyclohexanol by liquid phase oxidation of cyclohexane. Background technique [0002] The oxidation of cyclohexane to prepare cyclohexanone and cyclohexanol is an important industrial reaction, and most of the cyclohexanone and cyclohexanol in the world are produced by this method. Cyclohexanone and cyclohexanol are the main intermediates for the preparation of caprolactam and adipic acid to obtain nylon-6 and nylon-66, as well as important organic chemical raw materials and industrial solvents. [0003] At present, the liquid phase oxidation of cyclohexane in industrial production can be divided into two routes: non-catalytic oxidation and catalytic oxidation. [0004] The non-catalytic oxidation method uses oxygen-containing gas to oxidize cyclohexane to cyclohexyl hydrogen peroxide and a small amount of cyclohexanone and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/12C07C29/19C07C35/08C07C45/32C07C49/403
Inventor 李永祥王仲霞宗保宁闵恩泽
Owner CHINA PETROLEUM & CHEM CORP
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