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Method for directly preparing cyclohexanone from benzene

A cyclohexanone, direct technology, applied in the field of chemical technology, can solve the problems of high energy consumption, complex process and the like, achieve the effects of simple raw materials, simple product separation, and overcoming many reaction steps

Inactive Publication Date: 2016-04-27
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention aims at the disadvantages of complex technological process and high energy consumption in the current production process of cyclohexanone, and provides a method for directly preparing cyclohexanone from benzene. This method proposes to use benzene as raw material to directly synthesize cyclohexanone in one step for the first time. , a new method for the synthesis of pimelinketone, the concrete reaction process is shown in the following formula (1)
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Method used

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  • Method for directly preparing cyclohexanone from benzene
  • Method for directly preparing cyclohexanone from benzene
  • Method for directly preparing cyclohexanone from benzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In the autoclave, add benzene 20mmol, hydroxylamine salt 20mmol, NH 4 VO 3 (The first catalyst) 0.07g, the Pd / MCM-41 catalyst 0.3g (the second catalyst) that the load is 2% by mass percent, acetic acid 5ml, water 10ml (its molar ratio is 1:1:0.03:0.0028:4.37: 27.78) pass N 2Make a replacement. Then heat up to 80°C, keep the reaction for 1h, then feed hydrogen to the reaction pressure of 2MPa and keep for 3h, stop the hydrogen flow, cool down to room temperature, centrifuge the catalyst and the reaction solution, and the reaction solution is neutralized with a mass fraction of 30% NaOH solution, After toluene extraction and separation, the organic phase can be obtained, and the organic phase can be analyzed by gas chromatography. The yield of the product cyclohexanone was quantitatively calculated to be 6.84%.

Embodiment 2～4

[0034] Same as the operating steps and reaction conditions of the synthetic cyclohexanone process in Example 1, the first catalyst is changed to NaVO 3 (0.07g), Fe(NO) 3 (0.07g), V 2 o 5 / MCM-41 (0.1 g). The organic phase was analyzed by gas chromatography, and the yield of the product cyclohexanone was quantitatively calculated. The experimental results are shown in Table 1.

[0035] The impact of the first catalyst of table 1 on the synthetic cyclohexanone reaction

[0036]

[0037]

Embodiment 5～8

[0039] The operation steps and reaction conditions of the synthetic cyclohexanone process in Example 1 are the same, and the carrier of the second catalyst is changed to AC, γ-Al 2 o 3 , HZSM-5, SBA-15, etc. The organic phase was analyzed by gas chromatography, and the yield of the product cyclohexanone was quantitatively calculated. The experimental results are shown in Table 2.

[0040] The impact of the second catalyst carrier of table 2 on the synthetic cyclohexanone reaction

[0041] Example

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Abstract

The invention relates to a method for directly preparing cyclohexanone from benzene. The method comprises the following steps: putting benzene, hydroxylamine salt, a first catalyst, a second catalyst, Bronsted acid and water into a high-pressure reaction vessel, introducing N2 for displacement, heating to 60-150 DEG C and reacting for 0.5-3h; introducing hydrogen to 1-5 MPa, reacting for 1-6 h, cooling to room temperature, centrifuging to separate out catalysts and a reaction solution, and carrying out neutralization extraction separation on the reaction solution so as to obtain the product cyclohexanone. According to the invention, defects such as many reaction steps, complex separation process of products, high energy consumption and the like existing in a traditional cyclohexanone synthesis technology are overcome. The method has advantages as follows: the raw materials are simple and easily available; the synthesis process is simple; the reaction condition is mild; and product separation is simple. By one-time feeding, cyclohexanone can be produced by a benzene one-pot method, and yield of cyclohexanone reaches 12%.

Description

technical field [0001] The invention relates to a method for synthesizing cyclohexanone in one pot by using benzene, hydroxylamine salt and hydrogen as raw materials, belonging to the technical field of chemical technology. Background technique [0002] Cyclohexanone is the main intermediate for the preparation of nylon, caprolactam and adipic acid. It is also an important organic chemical raw material and industrial solvent. It is widely used in the fields of medicine, paint, coating, rubber and pesticides. [0003] At present, there are three main industrial production process routes of cyclohexanone: cyclohexane oxidation method, phenol hydrogenation method and cyclohexene hydration method, wherein more than 90% of cyclohexanone is produced by cyclohexane oxidation method. [0004] (1) cyclohexane oxidation method. The method can be divided into non-catalytic oxidation method and catalytic oxidation method. The non-catalytic oxidation method does not use a catalyst, but...

Claims

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Application Information

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IPC IPC(8): C07C45/00C07C49/403
CPCC07C45/00C07C49/403
Inventor 王延吉王彤张东升李志会徐元媛邬长城赵新强
Owner HEBEI UNIV OF TECH