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Method for directly preparing cyclohexanol from benzene

A cyclohexanol, direct technology, applied in the direction of hydroxyl addition preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of large equipment investment and high energy consumption, and achieve equipment investment The effect of less, high yield, and avoiding corrosion

Active Publication Date: 2013-04-10
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a method for directly preparing cyclohexanol from benzene. The method is to directly prepare cyclohexanol from benzene through selective hydrogenation and hydration in a batch reactor with dynamic control of reaction conditions. The method of hexanol overcomes the shortcomings of high energy consumption and large equipment investment due to the separation and purification of intermediate products in the current two-step process for preparing cyclohexanol from benzene

Method used

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  • Method for directly preparing cyclohexanol from benzene
  • Method for directly preparing cyclohexanol from benzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Add 15 ml of benzene, 30 ml of deionized water, 15 ml of ethylene glycol, 0.5 g of Ru-Zn / SiO to the reactor 2 (wherein the mass percent composition of Ru, Zn in the catalyst is 4% and 1% respectively) and 3 grams of HZSM-5 molecular sieves (purchased from Nankai University Catalyst Factory, SiO 2 / Al 2 o 3 The molar ratio is 25), sealed and then stirred, heated to 150° C., then filled with hydrogen into the reactor to make the partial pressure 5 MPa, and reacted for 30 minutes. A small amount of reaction liquid was taken out from the sampling valve and analyzed by gas chromatography. It can be seen that the conversion rate of benzene was 55.3%, and the yield of cyclohexene was 35.2%.

[0021] (2) After step (1), reduce the temperature of the reactor to 30°C within 10 minutes, discharge the gas in the reactor, and then replace it with nitrogen three times; fill the reactor with nitrogen to 0.5MPa; raise the temperature to 110°C , continue to react for 4 hours.

...

Embodiment 2～5

[0024] The consumption of ethylene glycol was changed, and the consumption of all the other chemical reagents, reaction steps and conditions were the same as in Example 1, and the reaction results were shown in Table 1.

[0025] The impact of the amount of ethylene glycol in table 1 on the direct preparation of cyclohexanol from benzene

[0026]

Embodiment 6

[0028] (1) Add 15 ml of benzene, 30 ml of deionized water, 15 ml of glycerol, 0.5 g of Ru-Zn / SiO to the reaction kettle 2 (wherein the mass percent composition of Ru, Zn in the catalyst is 4% and 1% respectively) and 3 grams of HZSM-5 molecular sieves (purchased from Nankai University Catalyst Factory, SiO 2 / Al 2 o 3 The molar ratio is 25), sealed and then stirred, heated to 150° C., then filled with hydrogen into the reactor to make the partial pressure 5 MPa, and reacted for 30 minutes. A small amount of reaction liquid was taken out from the sampling valve and analyzed by gas chromatography. It can be seen that the conversion rate of benzene was 65.8%, and the yield of cyclohexene was 30.7%.

[0029] (2) After step (1), reduce the temperature of the reactor to 30°C within 10 minutes, discharge the gas in the reactor, and then replace it with nitrogen three times; fill the reactor with nitrogen to 0.5MPa; raise the temperature to 110°C , continue to react for 4 hours.

...

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Abstract

The invention belongs to basic organic synthesis, and discloses a method for directly preparing cyclohexanol from benzene. The method comprises the following steps of: (1) adding benzene, deionized water, Ru series catalyst for benzene selective hydrogenation, cyclohexene hydration catalyst and additive into a reaction kettle, wherein the volume ratio of the benzene to the deionized water is 1:0.5-10, the molar ratio of Ru in the Ru series catalyst for benzene selective hydrogenation to the benzene is 1:200-2,000, the using amount of the cyclohexene hydration catalyst is 0.1 to 0.5 gram catalyst per millimeter benzene and the using amount of the additive is 0.5 to 2 millimeters additive per millimeter benzene; heating the mixture to between 100 and 200 DEG C, keeping the temperature, inflating hydrogen of which partial pressure is 2 to 7MPa into the reaction kettle, and reacting the mixture for 5 to 90 minutes; and (2) reducing the temperature of the reaction kettle to 30 DEG C, displacing the hydrogen in the kettle by using the nitrogen, inflating the nitrogen into the reaction kettle till the partial pressure of the nitrogen is 0.2 to 1MPa, and continuously reacting the mixture for 0.5 to 6 hours to obtain the cyclohexanol at the temperature of between 80 and 150 DEG C. The method has the advantages of low equipment investment, low production cost, easy operation and the like, reduces energy consumption, avoids corrosion on the reaction equipment in the absence of ZnSO4 additive, and obtains high cyclohexanol yield.

Description

technical field [0001] The invention belongs to basic organic synthesis, specifically a method for directly preparing cyclohexanol from benzene. The method is to directly prepare cyclohexanol from benzene through selective hydrogenation and hydration in a batch reactor with dynamic control of reaction conditions. Alcohol method. Background technique [0002] Cyclohexanol is an important saturated alicyclic alcohol, which is mainly used in the production of nylon 6 and nylon 66 raw materials - caprolactam and adipic acid. In addition, cyclohexanol can also be used in the fields of disinfectants, fragrances, insecticides, fungicides, leather softeners and wood preservatives. [0003] The methods for industrial production of cyclohexanol mainly include: ① hydrogenation of benzene to prepare cyclohexane, and then partial oxidation of cyclohexane with oxygen in the air to obtain cyclohexanol; ② partial hydrogenation of benzene to generate cyclohexene, and then cyclohexene Hexen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C35/08C07C29/04B01J29/40B01J23/60
Inventor 王延吉薛伟魏珺芳李芳赵新强
Owner HEBEI UNIV OF TECH