Regeneration method for Pd@CN catalyst for phenol hydrogenation

A catalyst and phenol technology, applied in the field of catalysis, can solve the problems of limited mass transfer, easy blockage of catalyst pores, low economic benefits, etc., and achieve the effect of restoring catalytic activity

Active Publication Date: 2018-12-04
NANJING MEMBRANE IND TECH RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The patent (publication number 104402687A) applied Pd@CN catalyst to phenol hydrogenation, and developed a new phenol hydrogenation process, but the concentration of phenol in this process is low, and the economic benefit is too low in the industrialization process
The patent (publication number 106861741A) increases the concentration of phenol, studies the hydrogenation process of phenol with water as the solvent under the concentration of 10% phenol, and develops a post-treatment method of phenol hydrogenation catalyst, which can solve the problem of 10% hydrogenation in the water system. % phenol concentration deactivation of Pd@CN catalyst, but as the phenol concentration continues to increase, the aqueous system is no longer suitable for the phenol hydrogenation process
Studies have shown that the hydrogenation process of high-concentration phenol shows better catalytic activity in the solvent cyclohexane, but the deactivation of the catalyst inevitably occurs, mainly due to the high concentration of organic matter in the hydrogenation process of high-concentration phenol, the organic matter Easier to block catalyst pores (most micropores), cover active sites, and limit mass transfer

Method used

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  • Regeneration method for Pd@CN catalyst for phenol hydrogenation
  • Regeneration method for Pd@CN catalyst for phenol hydrogenation

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Experimental program
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Effect test

Embodiment 1

[0025] The mixture after phenol hydrogenation reaction catalyzed by Pd@CN catalyst was filtered and separated to recover the catalyst. The recovered catalyst was placed in the reactor, a certain amount of cyclohexane was added, the reactor was sealed, and hydrogen was replaced 5 times. at 110 o C, 0.5 MPa, 500 rpm for 60 min. After the catalyst was recovered by filtration, it entered the next phenol hydrogenation activity test experiment, which was applied 10 times in total. The change of catalytic performance of Pd@CN catalyst is as follows: figure 2 shown. The conversion rate and selectivity of phenol remained basically unchanged, showing good stability.

Embodiment 2

[0027] The mixture after the phenol hydrogenation reaction catalyzed by the Pd@CN catalyst was filtered and separated to recover the catalyst. The recovered catalyst was placed in a reactor, a certain amount of water was added, the reactor was sealed, and nitrogen replacement was used for 5 times. at 80 o C, 0.1MPa, 100 rpm washing for 30 min. After the catalyst was recovered by filtration, it entered the next phenol hydrogenation activity test experiment, which was applied 10 times in total. The results showed that the selectivity of cyclohexanone remained basically unchanged, and the conversion of phenol decreased by about 15%.

Embodiment 3

[0029] The mixture after phenol hydrogenation reaction catalyzed by Pd@CN catalyst was filtered and separated to recover the catalyst. The recovered catalyst was placed in the reactor, a certain amount of ethanol was added, the reactor was sealed, and replaced with argon 5 times. at 140 o C, wash at 1.5 MPa, 300 rpm for 90 min. After the catalyst was recovered by filtration, it entered the next phenol hydrogenation activity test experiment, which was applied 10 times in total. The results showed that the selectivity of cyclohexanone remained basically unchanged, and the conversion of phenol decreased by about 25%.

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PUM

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Abstract

The invention relates to a regeneration method for a Pd@CN catalyst for phenol hydrogenation. The regeneration method comprises the following steps: after the Pd@CN catalyst is used to catalyze the phenol hydrogenation, the catalyst is recovered by filtration, the recovered catalyst is placed into a reaction kettle, a solvent is added, washing is performed under certain conditions to regenerate the catalyst, and after secondary filtration is performed, the obtained catalyst is used for a next application experiment. The regeneration method provided by the invention can effectively regenerate the deactivated catalyst, realize the recycling of the catalyst, reduce a use amount of the catalyst, improve economic efficiency of the process, and provide a guarantee for the green production process of preparing cyclohexanone by the phenol hydrogenation.

Description

technical field [0001] The invention relates to a regeneration method of a Pd@CN catalyst, in particular to a regeneration method of a Pd@CN catalyst in a high-concentration phenol hydrogenation process, and belongs to the technical field of catalysis. Background technique [0002] The downstream products of cyclohexanone, caprolactam and adipic acid, are important intermediates for the synthesis of nylon 6 and nylon 66. The main production process of cyclohexanone in industry is the cyclohexane oxidation method, but this method has many by-products, more acid-containing wastewater, and greater environmental pollution. In recent years, the one-step hydrogenation of phenol to cyclohexanone has attracted much attention due to its short process flow and high atom utilization. [0003] The patent (publication number 104402687A) applied Pd@CN catalyst to phenol hydrogenation and developed a new phenol hydrogenation process. However, the concentration of phenol in this process is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/28B01J27/24B01J38/58B01J38/48B01J38/52
CPCB01J27/24B01J27/28B01J38/48B01J38/52B01J38/58
Inventor 陈日志屈正炎郭百涛邢卫红
Owner NANJING MEMBRANE IND TECH RES INST CO LTD
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