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Method for preparing adipate

A technology for adipic acid and cyclohexane, which is applied in the field of one-step preparation of adipic acid by catalytic oxidation of cyclohexane, can solve the problem of high cost, and achieve the effects of low cost, low reaction temperature and pressure, and good selectivity

Active Publication Date: 2014-04-02
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Wang Y et al. (Angew Chem Int Edit 2010, 49, 3356-3359) reported a method for catalyzing the oxidation of cyclohexane using porous carbon doped with N and B. However, the method requires the use of H 2 o 2 As an oxidizing agent, the cost is relatively high, and the main products are cyclohexanone and cyclohexanol

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preparation example Construction

[0039] Nitrogen-doped activated carbon preparation method, the specific steps are as follows:

[0040] (1) Activated carbon is first soaked in 2mol / L hydrochloric acid at 80°C for 2 hours, then soaked in 1mol / L hydrofluoric acid at room temperature for 24 hours, then washed with distilled water until neutral, dried and heat-treated at 1000°C in Ar atmosphere for 2 hours, After natural cooling, screen out activated carbon with a diameter of 40-60 mesh;

[0041] (2) The activated carbon treated in step (1) was heated to 500 °C in an Ar atmosphere, and then NH 3 , NH 3 Flow accounted for NH 3 and 20% of the total flow of Ar, was treated at a constant temperature for 1 h, and cooled to room temperature in an Ar atmosphere to obtain nitrogen-doped activated carbon. The doping amount of nitrogen is about 2% (mass fraction).

[0042] Preparation method of nitrogen-doped carbon nanotubes:

[0043] (1) Preparation of Fe-Mo / Al by co-precipitation method 2 o 3 Catalyst: Ferric nit...

Embodiment 1

[0048] 94g of cyclohexane, 2.7g of cyclohexanone, 62.6g of acetone, and 0.2g of nitrogen-doped activated carbon were added into a closed reaction kettle and mixed to form a mixed suspension. The mixed suspension was heated to 125°C under stirring, and oxygen was fed to 1.5Mpa, and the temperature and pressure were kept constant. After 8 hours of reaction, it was cooled to room temperature, and the liquid-solid phase mixture was taken out, and it was filtered to obtain a solid catalyst (nitrogen doped activated carbon) and a liquid phase mixture containing unreacted reactants and reaction products.

[0049] The above liquid phase mixture was analyzed to determine the conversion and selectivity of the reaction. The analysis method is carried out according to the method disclosed in the patent CN1936586A, wherein the analysis of cyclohexane, cyclohexanone and cyclohexanol is carried out on the Agilent 6820 gas chromatograph equipped with a capillary column, and the analysis of ad...

Embodiment 2

[0051] 94g of cyclohexane, 9.4g of cyclohexanone, 62.6g of acetone, and 9.4g of nitrogen-doped activated carbon were added into a closed reaction kettle and mixed to form a mixed suspension. The mixed suspension was heated to 200°C under stirring, and oxygen was fed to 5Mpa, and the temperature and pressure were kept constant. After 8 hours of reaction, it was cooled to room temperature, the liquid-solid phase mixture was taken out, and it was filtered to obtain a solid catalyst (nitrogen doped heterogeneous activated carbon) and a liquid phase mixture containing unreacted reactants and reaction products.

[0052] The above liquid phase mixture was analyzed to determine the conversion and selectivity of the reaction. The analysis method is carried out according to the method disclosed in the patent CN1936586A, wherein the analysis of cyclohexane, cyclohexanone and cyclohexanol is carried out on the Agilent 6820 gas chromatograph equipped with a capillary column, and the analys...

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Abstract

The invention discloses a method for preparing adipate, comprising the following steps of: (1) adding cyclohexane, solvent, an initiator and a solid catalyst into a reactor and mixing to form a mixed suspension; (2) introducing enough amount of oxygen into the mixed suspension to be used as an oxidant; and reacting under the conditions that the pressure is 0.5-5MPa and the temperature is 100-200DEG C for 1-20h; (3) separating the reaction mixture in the step (2) to obtain the solid catalyst and a liquid phase mixture; and (4) separating the adipate from the liquid phase mixture in the step (3). The invention prevents nitric acid from corroding the environment and the equipment, can solve the problems that a homogeneous catalyst is difficult to recover and is deactivated in the oxidation process of the cyclohexane, is free from using noble metals and has high reaction selectivity and favorable activity. The used catalyst can be recycled.

Description

technical field [0001] The invention relates to a method for preparing adipic acid, in particular to a method for preparing adipic acid in one step through catalytic oxidation of cyclohexane. Background technique [0002] Adipic acid is an important raw material for the preparation of polyurethane and nylon 66, and is also an intermediate for many lubricating oil additives. In the traditional adipic acid production process, benzene is mainly used as the starting material, and cyclohexane is first produced by hydrogenation, and then cyclohexane is oxidized into cyclohexanol and cyclohexanone (KA oil), and then KA is decomposed with nitric acid The oil is oxidized to adipic acid. [0003] The first step of the above process is to oxidize cyclohexane to produce cyclohexanol and cyclohexanone. Homogeneous cobalt-based catalysts (ZL 94110939.9) are often used. The catalysts are difficult to separate and recover, and will cause slagging in the pipeline. In order to control the s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/14C07C51/31
CPCY02P20/584
Inventor 余皓彭峰谈俊王红娟
Owner SOUTH CHINA UNIV OF TECH
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