Preparation method of hydrogenation catalyst and method for preparing cyclohexanone through phenol selective hydrogenation

A hydrogenation catalyst and catalyst technology, which is applied in the preparation of organic compounds, the hydrogenation preparation of aromatic hydroxyl compounds, and the preparation of carbon-based compounds, etc., to achieve the effects of short production cycle, good dispersibility, and simple preparation methods

Active Publication Date: 2017-05-10
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present, there is no Pd-La with good hydrogenation effect in this field. 2 o 3 /activated c

Method used

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  • Preparation method of hydrogenation catalyst and method for preparing cyclohexanone through phenol selective hydrogenation
  • Preparation method of hydrogenation catalyst and method for preparing cyclohexanone through phenol selective hydrogenation

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Add activated carbon to 10% dilute nitric acid, heat and reflux in a water bath at 60°C for 2 hours, filter, wash with deionized water until there is no chloride ion, and dry at 120°C to obtain acid-treated activated carbon. Take 0.554gLa(NO 3 ) 3 ·nH 2 O was dissolved in 120mL deionized water and stirred until La(NO 3 ) 3 ·nH 2 O is completely dissolved, add 5 g of acid-treated activated carbon, continue to stir, and use 0.4 mol / L NH 4 HCO 3 Adjust the pH of the solution to 7, put the solution into a microwave reactor, and react with 400W for 30s and 30s for a total of 16 minutes, so the microwave irradiation time is 8 minutes. The obtained solution is washed with absolute ethanol and deionized water, filtered, and dried at 70°C. After calcination at 700℃, La 2 o 3 Mass fraction of 10% La 2 o 3 / AC carrier. Take 0.582gLa 2 o 3 / AC dispersed in 100mL deionized water, add 5mL methanol, 1.5mL chloropalladium acid solution, ultrasonically disperse for 30min, t...

Embodiment 2

[0042] With embodiment 1, the difference is that Pd-La 2 o 3 The mass fraction of Pd in ​​ / AC is 2%, that is, 2%Pd-10%La 2 o 3 / AC.

Embodiment 3

[0044] With embodiment 1, the difference is that Pd-La 2 o 3 The mass fraction of Pd in ​​ / AC is 1%, that is, 1%Pd-10%La 2 o 3 / AC.

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PUM

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Abstract

The invention provides a preparation method of a hydrogenation catalyst. The catalyst is a Pd-La2O3/activated carbon catalyst. The preparation method comprises the following steps: A, pretreating activated carbon; B, preparing a La2O3/activated carbon composite carrier: dissolving lanthanum salt into water and/or ethanol, mixing the solution and the activated carbon subjected to acid treatment, adjusting the pH value of the formed mixed solution to be 5.5 to 8.5, putting the solution with the pH value adjusted into a microwave device, performing microwave irradiation reaction, and performing washing, solid-liquid separation, drying and calcinations on the obtained product to obtain the La2O3/activated carbon composite carrier; and C, preparing a Pd-La2O3/activated carbon catalyst: dispersing the composite catalyst into water, mixing the composite carrier dispersed into water, methanol and a chloropalladic acid solution, performing photoreduction on the obtained mixed solution under ultraviolet light, and performing solid-liquid separation and drying on the obtained product to obtain the Pd-La2O3/activated carbon catalyst. The hydrogenation catalyst provided by the invention is particularly suitable for catalysis of phenol selective hydrogenation to prepare cyclohexanone.

Description

technical field [0001] The present invention relates to the field of catalyst preparation methods, in particular to a preparation method of a novel nanocomposite hydrogenation catalyst, the hydrogenation catalyst prepared by the method, and the application of the hydrogenation catalyst in the preparation of cyclohexanone by selective hydrogenation of phenol , and a method for the selective hydrogenation of phenol to cyclohexanone. Background technique [0002] Cyclohexanone is an important raw material for the monomer caprolactam and adipic acid of synthetic fibers nylon 6 and nylon 66, and is also an important intermediate for fine chemicals such as medicine, coatings and dyes. The preparation of cyclohexanone mainly includes cyclohexane oxidation and phenol hydrogenation. The former has high reaction requirements, high temperature and high pressure, high energy consumption, and low conversion rate, while the latter is increasingly favored because of its simple operation a...

Claims

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Application Information

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IPC IPC(8): B01J23/63C07C45/00C07C49/403
CPCB01J23/63C07C45/006C07C49/403
Inventor 周继承张燕吉王非
Owner XIANGTAN UNIV
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