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Cosynthesis device and method of cyclohexanol, cyclohexanone and adipic acid in microchannels

A synthesis device and technology for cyclohexanol, which are applied in chemical instruments and methods, preparation of carboxylic acids by oxidation, preparation of peroxy compounds, etc., can solve the problems of low selectivity between cyclohexanol and cyclohexanone, low conversion rate of cyclohexane, Environmental pollution and other problems, to achieve the effect of improving conversion rate and selectivity, shortening reaction time, and eliminating potential safety hazards

Inactive Publication Date: 2012-10-24
ZHEJIANG UNIV
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  • Application Information

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Problems solved by technology

[0007] In short, the current cyclohexane oxidation production process has low conversion rate of cyclohexane, low selectivity of cyclohexanol and cyclohexanone, a large amount of unreacted cyclohexane needs to be recycled, high energy consumption, serious environmental pollution, and Potential safety hazards of oxidation explosions and other issues

Method used

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  • Cosynthesis device and method of cyclohexanol, cyclohexanone and adipic acid in microchannels
  • Cosynthesis device and method of cyclohexanol, cyclohexanone and adipic acid in microchannels
  • Cosynthesis device and method of cyclohexanol, cyclohexanone and adipic acid in microchannels

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Experimental program
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Effect test

Embodiment 1

[0021] The reaction microtube is 35m in length and 0.508mm in inner diameter, rolled into a ring with a diameter of 20cm and placed in an air thermostat. The reaction temperature is 180°C, the pressure is 1.5MPa, the molar ratio of oxygen to cyclohexane is 0.3:1, the flow rate of cyclohexane is 0.79mL / min, the flow rate of the oxygen mass flow controller is set to 49.38mL / min, and the flow rate of isopropanol The flow rate is set to 0.8mL / min. After the reaction is stable, the cyclohexanol and cyclohexanone in the liquid phase product are analyzed by gas chromatography, the intermediate product cyclohexyl hydroperoxide is analyzed by iodine titration, and diacids such as adipic acid The by-products were analyzed by alkali titration. After inspection, the conversion rate of cyclohexane under this condition is 3.10%, the selectivity sum of cyclohexanol and cyclohexanone is 51.83%, the selectivity of cyclohexyl hydroperoxide is 30.17%, and the selectivity of adipic acid is 1...

Embodiment 2

[0023]The reaction microtube is 35m in length and 0.508mm in inner diameter, rolled into a ring with a diameter of 20cm and placed in an air thermostat. The reaction temperature is 200°C, the pressure is 8 MPa, the molar ratio of oxygen to cyclohexane is 0.15:1, the flow rate of cyclohexane is 2.36 mL / min, the flow rate of oxygen mass flow controller is 74.08 mL / min, and the flow rate of isopropanol is 1 mL / min. Under these conditions, the conversion rate of cyclohexane is 10.10%, the selectivity sum of cyclohexanol and cyclohexanone is 66.93%, the selectivity of cyclohexyl hydroperoxide is 8.78%, and the selectivity of adipic acid is 24.29% %.

Embodiment 3

[0025] For the cyclohexane oxidation reaction in the micro-reaction tube, the residence time is defined as the apparent residence time of cyclohexane at normal temperature, that is, the ratio of the volume of the empty tube to the volume flow rate of cyclohexane at normal temperature. The conversion rate of cyclohexane to cyclohexanol, cyclohexanone and adipic acid and the distribution of products are different under different residence times.

[0026] The residence time is 4 minutes: the reaction microtube is 35 m long and 0.508 mm in inner diameter, rolled into a ring with a diameter of 20 cm and placed in an air incubator. The reaction temperature is 180°C, the pressure is 1.5MPa, the molar ratio of oxygen to cyclohexane is 0.5:1, the flow rate of cyclohexane is 1.77mL / min, the flow rate of oxygen mass flow controller is set to 185.19mL / min, and the flow rate of isopropanol is 1mL / min. Under these conditions, the conversion rate of cyclohexane is 0.62%, the selectivity su...

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Abstract

The invention discloses a cosynthesis device and method of hexanol, cyclohexanone and adipic acid in microchannels. The method comprises the steps of mixing and preheating cyclohexane and oxygen or air by a gas-liquid micro mixer, entering a micro reaction tube in an air thermostat, and reacting, wherein the cyclohexane flow is controlled by a laminar flow pump, the oxygen or air flow is controlled by a mass flow controller, the cyclohexane flow and the oxygen or air flow are kept at a certain ratio, and the reaction pressure is controlled by a back pressure valve; and separating the reaction product by a gas-liquid micro separator, collecting the liquid-phase product by a storage tank, and discharging the gas phase. According to the invention, continuous production of cyclohexanol, cyclohexanone and adipic acid is realized; because the gas-liquid micro mixer, the micro reaction tube, and the gas-liquid micro separator are adopted, the specific surface area of the fluid passing through the channels is large, heat transfer effect of mixing, reaction, separation and other processes is good, pure oxygen and air can be used as an oxidant in the reaction, operation can be carried out at higher reaction pressure and reaction temperature, the reaction safety is greatly improved, and the selectivity and conversion rate are greatly improved.

Description

technical field [0001] The invention relates to a co-synthesis device and method for cyclohexanol, cyclohexanone and adipic acid in a microchannel. Background technique [0002] Cyclohexanone and cyclohexanol (commonly known as KA oil) are important chemical raw materials. Million tons of cyclohexanol and cyclohexanone are obtained by oxidation of cyclohexane every year. In addition to being mainly used for the synthesis of caprolactam and adipic acid, In addition to synthesizing nylon-6 and nylon-66, it can also be directly used as a solvent. [0003] The vast majority of cyclohexanol and cyclohexanone in the world are obtained through the liquid phase oxidation of cyclohexane, which can be divided into two production routes: non-catalyzed oxidation and catalytic oxidation. [0004] The non-catalyzed oxidation method, also known as the peroxide oxidation method, was first successfully developed by the French Rhone-Poulenc company. The characteristic of the non-catalyzed o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C27/12C07C35/08C07C29/50C07C49/403C07C45/33C07C55/14C07C51/31C07C407/00C07C409/14
Inventor 朱明乔王磊卢建刚张红光胡红定葛倩
Owner ZHEJIANG UNIV
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