Method for directly producing adipic acid by cyclohexane catalytic oxidation

A technology of catalytic oxidation and cyclohexane, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve the problem of high cost, achieve short route, high catalytic activity, easy separation and recycling Effect

Inactive Publication Date: 2011-04-06
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst is ruthenium oxide supported by a solid carrier, and the solid carrier is alumina, molecular sieve, carbon nanotube, silica, activated carbon, zeolite, sepiolite, porous ceramic or polyvinyl chloride; the catalyst has high catalytic efficiency and stability Good, but using nano-ruthenium dioxide noble metal catalyst, the cost is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 237g of cyclohexane, acetone, tert-butyl hydroperoxide and multi-walled carbon nanotubes into a closed reaction kettle and mix to form a mixed suspension. Wherein, the weight ratio of acetone to cyclohexane is 1:1.5, the weight ratio of cyclohexane to multi-walled carbon nanotubes is 474:1, and the weight ratio of cyclohexane to tert-butyl hydroperoxide is 34:1. The suspension is heated to 125°C under stirring, and oxygen is introduced to 1.5MPa. Since the reaction process continuously consumes oxygen in a stoichiometric ratio, oxygen is continuously supplemented through a pressure stabilizing device and a flow meter connected to an oxygen source during the reaction. And keep the pressure constant at 1.5MPa. After reacting for 8 hours, discharge the liquid-solid phase mixture from the bottom of the reaction kettle, filter it to obtain a solid catalyst and a liquid phase mixture, and analyze the liquid phase mixture to determine the conversion rate and selectivity of...

Embodiment 2～4

[0023] Add 237g of cyclohexane, acetone, cyclohexanone and multi-walled carbon nanotubes into a closed batch reactor and mix to form a mixed suspension. Wherein, the weight ratio of acetone to cyclohexane is 1:1.5, the weight ratio of cyclohexane to multi-walled carbon nanotubes is 474:1, and the weight ratio of cyclohexane to cyclohexanone is 40:1. The mixed suspension was heated to the temperature shown in Table 1 respectively under stirring, and oxygen was introduced to 1.5 MPa, and oxygen was constantly supplemented during the reaction and the pressure was kept constant at 1.5 MPa. After reacting for 8 hours, discharge the liquid-solid phase mixture from the bottom of the reaction kettle, filter it to obtain a solid catalyst and a liquid phase mixture, and analyze the liquid phase mixture to determine the conversion rate and selectivity of the reaction. The separation and analysis methods of the product are the same as in Example 1, and adipic acid with a purity of 99.1%, ...

Embodiment 5

[0028] 237g of cyclohexane and the corresponding amount of acetone, cyclohexanone and multi-walled carbon nanotubes were added into a closed batch reactor and mixed to form a mixed suspension. Wherein, the weight ratio of solvent to cyclohexane is 1:1.5, the weight ratio of cyclohexane to multi-walled carbon nanotubes is 474:1, and the weight ratio of cyclohexane to cyclohexanone is 40:1. The mixed suspension was heated to 125°C under stirring, and oxygen was fed to 1MPa, and reacted for 8 hours. The separation and analysis method of the product was the same as in Example 1. The conversion rate of cyclohexane was 21%, and the selectivity of adipic acid was 28%. .

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Abstract

The invention discloses a method for directly producing adipic acid by catalytically oxidizing cyclohexane, which comprises the following steps: mixing cyclohexane, a solvent, an initiator and a carbon catalyst to form a mixed suspension, wherein the weight ratio of the solvent, the carbon catalyst, the initiator and cyclohexane is (0 to 99):(0.1 to 0.000125):(1 to 0.0005):1, and the carbon catalyst is carbon nanotube, graphite or active carbon; heating the mixed suspension to 50 to 250 DEG C; introducing oxygen or air as an oxidant; keeping the pressure in a reaction kettle at 0.1 to 5 MPa, and reacting for 0.1 to 20 h; and separating the reaction mixture to obtain the adipic acid product. The method can prevent environment pollution and corrosion of equipment due to the use of nitric acid, and can solve the problems such as the difficulties in recovering the homogeneous catalyst and deactivation of the homogeneous catalyst in the oxidization process of cyclohexane. No noble metal catalyst is used to reduce the catalyst cost, and the used catalyst can be recovered and used repeatedly.

Description

technical field [0001] The invention relates to a method for producing adipic acid, in particular to a method for directly producing adipic acid through catalytic oxidation of cyclohexane. Background technique [0002] Adipic acid is an important chemical intermediate and an important raw material for the preparation of polyurethane and nylon 66. In the traditional adipic acid production process, the first step is to oxidize cyclohexane to generate cyclohexanol and cyclohexanone (KA oil), the conversion rate is generally <10%, and the selectivity is 70-90%. The product separation consumes a lot of energy and produces A large amount of waste lye; in the second step, nitric acid is used to oxidize KA oil into adipic acid, and nitrogen oxides that seriously pollute the environment are produced during the production process, which severely corrodes the equipment and requires harsh operating conditions. Therefore, the development of a new method for the production of adipic a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/215B01J21/18C07C55/14
CPCY02P20/584
Inventor 彭峰吴春玲余皓王红娟
Owner SOUTH CHINA UNIV OF TECH
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