Carbon deposition deactivated noble metal loading type catalyst regeneration method

A supported catalyst and precious metal technology, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc. Growth, good regeneration effect, avoid the effect of sintering

Inactive Publication Date: 2005-12-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is that in the prior art, during the regeneration process of the noble metal supported catalyst deactivated by carbon deposits, the air carbon burning method usually used is likely to cause the sintering of the noble metal and the growth of the metal particles, resulting in the permanent catalyst. In order to solve the problem of deactivation, a new regeneration method for noble metal-supported catalysts deactivated by regenerating carbon deposits is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] At a reaction temperature of 220°C, a reaction pressure of 1.5MPa, and a liquid hourly space velocity of 0.3 hours -1 , NH 3 / 2, 6-DIPP (mol) = 10, H 2 Carry out 2 under / 2,6-DIPP (mol)=20, the Pd (0.5% by weight)-La (0.25% weight) / spinel catalyst, keep the temperature constant at 220°C, stop feeding 2,6-diisopropylphenol and liquid ammonia, and increase the hydrogen gas phase space velocity to 600 hours -1 (volume), process the deactivated catalyst for 48 hours, then feed 2,6-diisopropylphenol and liquefied ammonia to reduce the hydrogen flow rate to the reaction conditions and react again. After regeneration by hydrogen treatment, the catalytic activity of the catalyst was recovered from 94.2% conversion of 2,6-diisopropylphenol to 95.7% of fresh catalyst activity, and the selectivity of 2,6-diisopropylaniline was recovered from 82.5% 95.0% selectivity to fresh catalyst.

Embodiment 2

[0011] At a reaction temperature of 220°C, a reaction pressure of 1.5MPa, and a liquid hourly space velocity of 0.6 hours -1 , NH 3 / 2, 6-DIPP (mol) = 10, H 2 Pd (0.5% by weight)-La (0.1% by weight) / spinel catalyst after 116 hours of deactivation of 2,6-diisopropylphenol vapor phase amination reaction under / 2,6-DIPP (mol)=20 , keep the temperature at 220°C, stop feeding 2,6-diisopropylphenol and liquid ammonia, and increase the hydrogen gas phase space velocity to 1000 hours -1 (volume), process the deactivated catalyst for 24 hours, then feed 2,6-diisopropylphenol and liquefied ammonia to reduce the hydrogen flow rate to the reaction conditions and react again. After regeneration by hydrogen treatment, the catalytic activity of the catalyst was recovered from 93.6% conversion of 2,6-diisopropylphenol to 97.3% of fresh catalyst activity, and the selectivity of 2,6-diisopropylaniline was recovered from 83.7% The selectivity to fresh catalyst was 97.8%.

Embodiment 3

[0013] At a reaction temperature of 220°C, a reaction pressure of 1.5MPa, and a liquid hourly space velocity of 0.6 hours -1 , NH 3 / 2, 6-DIPP (mol) = 10, H 2 Pd (0.5% by weight)-La (0.1% by weight) / spinel catalyst after 100 hours deactivation of 2,6-diisopropylphenol vapor phase amination reaction under / 2,6-DIPP (mol)=20 , stop feeding 2,6-diisopropylphenol and liquid ammonia, and increase the hydrogen gas phase space velocity to 1000 hours at a temperature of 300°C -1 (volume), process the deactivated catalyst for 24 hours, then feed 2,6-diisopropylphenol and liquefied ammonia to reduce the hydrogen flow rate to the reaction conditions and react again. After regeneration by hydrogen treatment, the catalytic activity of the catalyst was recovered from 95.2% conversion of 2,6-diisopropylphenol to 99.1% of fresh catalyst activity, and the selectivity of 2,6-diisopropylaniline was recovered from 81.5% The selectivity to fresh catalyst was 95.8%.

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Abstract

A process for regenerating the carried noble metal catalyst deactivated by carbon deposit, in order to use it in preparing 2,6-biisopropyl phenylamine features that the H2, CO, or their mixture is used to eliminate the carbon deposit from said catalyst.

Description

technical field [0001] The invention relates to a method for regenerating a precious metal-supported catalyst deactivated by carbon deposition, in particular to a palladium-supported catalyst for preparing 2,6-diisopropylaniline by gas-phase amination of 2,6-diisopropylphenol deactivated by carbon deposition regeneration method. Background technique [0002] 2,6-Diisopropylaniline is an important organic chemical intermediate, mainly used in pesticides, medicines, dyes, epoxy resin curing agents, food additives, etc. As early as the 1950s, Bayer Company carried out research on the liquid-phase alkylation of aniline, which required high temperature and high pressure. In 1987, the aniline gas-phase alkylation method developed by Air Products and Chemicals Company used molecular sieve catalysts, and the product selectivity was poor. In 1981, Nobert (DE3425629) of BASF Company developed the gas-phase amination method of phenolic compounds to prepare...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J37/18C07C209/10C07C211/46
CPCY02P20/584
Inventor 谢在库陈庆龄姜瑞霞陆贤
Owner CHINA PETROLEUM & CHEM CORP
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