Regeneration method for modified zeolite molecular sieve amination catalyst

A modified zeolite and catalyst technology, applied in molecular sieve catalysts, catalyst regeneration/reactivation, physical/chemical process catalysts, etc., to achieve the effect of solving carbon deactivation, reducing diffusion resistance, and prolonging service life

Active Publication Date: 2013-03-20
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a regeneration treatment method of a modified zeolite molecular sieve amination catalyst, overcome the above-mentioned deficiencies in the background technology, solve the problem of hydrothermal dealumination and deactivation of the modified zeolite molecular sieve amination catalyst, and improve the use of the catalyst life

Method used

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  • Regeneration method for modified zeolite molecular sieve amination catalyst
  • Regeneration method for modified zeolite molecular sieve amination catalyst
  • Regeneration method for modified zeolite molecular sieve amination catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 1. Modified zeolite molecular sieve amination catalyst regeneration treatment method

[0028] a) Add the deactivated modified zeolite molecular sieve amination catalyst into deionized water according to the solid-to-liquid ratio of 1:4, slowly add an appropriate amount of citric acid under strong stirring until the pH value of the reaction suspension reaches 4-5, and heat to reflux 2h, filter, wash to neutral, and dry.

[0029] b) The coke-dissolving modified zeolite molecular sieve amination catalyst obtained in step a) is used at 260° C. 2 / O 2 The mixed gas is used for low-temperature charcoal regeneration, and the exothermic temperature difference in the process of regeneration charcoal is controlled to be ≤5°C until no CO is detected in the reaction tail gas. 2 generated, the temperature is raised to 400°C to continue to use N 2 / O 2 The mixed gas is used for high-temperature charcoal regeneration, and the exothermic temperature difference in the regeneration c...

Embodiment 2

[0037] 1. Modified zeolite molecular sieve amination catalyst regeneration treatment method

[0038] a) Add the deactivated modified zeolite molecular sieve amination catalyst into deionized water according to the solid-to-liquid ratio of 1:4, slowly add an appropriate amount of oxalic acid under strong stirring until the pH value of the reaction suspension is 4-5, heat and reflux for 2 hours , filtered, washed to neutral, and dried.

[0039] b) The coke-dissolving modified zeolite molecular sieve amination catalyst obtained in step a) is regenerated at 260° C. using a mixed gas of N2 / O2 to burn charcoal at a low temperature, and control the exothermic temperature difference in the process of regenerated charcoal ≤ 5° C. to No CO detected in the reaction tail gas 2 generated, the temperature is raised to 400°C to continue to use N 2 / O 2 The mixed gas is used for high-temperature charcoal regeneration, and the exothermic temperature difference in the regeneration charcoal b...

Embodiment 3

[0047] 1. Modified zeolite molecular sieve amination catalyst regeneration treatment method

[0048] a) Add the deactivated modified zeolite molecular sieve amination catalyst into deionized water according to the solid-to-liquid ratio of 1:4, slowly add an appropriate amount of malic acid under vigorous stirring until the pH value of the reaction suspension reaches 4-5, and heat to reflux 2h, filter, wash to neutral, and dry.

[0049] b) The coke-dissolving modified zeolite molecular sieve amination catalyst obtained in step a) is used at 260° C. 2 / O 2 The mixed gas is used for low-temperature charcoal regeneration, and the exothermic temperature difference in the process of regeneration charcoal is controlled to be ≤5°C until no CO is detected in the reaction tail gas. 2 generated, the temperature is raised to 400°C to continue to use N 2 / O 2 The mixed gas is used for high-temperature charcoal regeneration, and the exothermic temperature difference in the regeneration ...

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Abstract

The invention discloses a regeneration treatment method for a modified zeolite molecular sieve amination catalyst. The regeneration method comprises the following steps of: regenerating soluble coke by inorganic acid or organic acid; smelting most coking materials and non-framework aluminum formed by hydrothermal dealumination; and performing charking regeneration on the smelted zeolite molecular sieve amination catalyst by N2 and O2 mixed gas to completely remove non-smelted coke, so that the performance of the modified zeolite molecular sieve amination catalyst is recovered. By the regeneration treatment method, the problem of activity loss caused by the hydrothermal dealumination is solved; and the service life of the modified zeolite molecular sieve amination catalyst is prolonged. The regeneration treatment method is mainly applied to a regeneration treatment process of the modified zeolite molecular sieve amination catalyst under the ethanol amine and the ammonia condensation and amination reaction.

Description

technical field [0001] The invention relates to a regeneration treatment method of a catalyst, in particular to a regeneration treatment method of a modified zeolite molecular sieve amination catalyst for the gas phase condensation amination reaction of ethanolamine and ammonia. Background technique [0002] The modified zeolite molecular sieve amination catalyst has been widely used in the gas phase condensation amination reaction of ethanolamine and ammonia under high temperature and high pressure conditions. [0003] The common problems of this kind of modified zeolite molecular sieve amination catalysts are: firstly, because the reactants and various reaction products are strongly alkaline substances, it is easy to adsorb and difficult to desorb at various acidic sites of the modified zeolite molecular sieve catalysts. Attached, it is easy to further react to generate various basic coking compounds, block the catalyst pores, cover the active sites of the catalyst, and ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/90B01J38/62B01J38/60B01J38/20C07B43/04
CPCY02P20/584
Inventor 赵锋伟吕剑杨建明余秦伟王伟梅苏宁魏阿宝李亚妮李春迎
Owner XIAN MODERN CHEM RES INST
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