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Regeneration method of catalyst for producing diphenylamine with phenylamine continuous condensation

A catalyst and diphenylamine technology, which is applied in the field of regeneration of diphenylamine catalyst prepared by continuous condensation of aniline, can solve the problem of a regeneration method without deactivation of the catalyst, and achieve the effects of preventing flying temperature, flexible process switching and short regeneration time.

Active Publication Date: 2008-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no regeneration method for this type of deactivated catalyst in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The catalyst composition is as follows: 70wt% Hβ zeolite (SiO 2 / Al 2 o 3 The molar ratio is 67), the alkaline earth metal Ba accounts for 1.5wt% of the catalyst, and the rest is γ-Al 2 o 3 .

[0028] According to the method of patent CN1289642A, 100 g of catalyst was prepared, numbered D-1. Reaction temperature 300~350℃; pressure 2.0MPa; space velocity 0.6h -1 The reaction of preparing diphenylamine by continuous condensation of aniline is carried out under the process conditions. When the conversion rate of aniline is less than 15% (mol), the catalyst is regarded as deactivated, and the production is shut down according to the shutdown plan to prepare for catalyst regeneration.

Embodiment 2

[0030] Regeneration in the reactor is adopted, the regeneration temperature in step (a) is controlled below 300°C, the regeneration temperature in step (b) is below 425°C, the regeneration temperature in step (c) is below 470°C, and the regeneration temperature in step (d) is Below 470°C.

[0031] First purging the deactivated catalyst D-1 with nitrogen, the process is as follows: under the system pressure of 2.0 MPa, purging with nitrogen according to the gas-to-solvent ratio of 40 (V) until there is no reaction mixture in the tail gas, and detect with gas chromatography.

[0032] The step-by-step combustion regeneration process with oxygen-containing nitrogen is as follows:

[0033] (a) Raise the temperature in the preheating section of the reactor inlet to 220°C at a rate of 15°C / h, and at the same time switch the nitrogen gas to oxygen-containing nitrogen, the oxygen content is 0.15v%, and after the catalyst bed has no temperature rise, the constant temperature time is 4 h...

Embodiment 3

[0042] The catalyst composition is as follows: 82.3wt% Hβ zeolite (SiO 2 / Al 2 o 3 The molecular ratio is 68), the alkali metal K accounts for 2.05wt% of the catalyst, and the rest is γ-Al 2 o 3 .

[0043] According to the patent CN200510047489.9 method to prepare catalyst 100g, number D-2. Reaction temperature 300~350℃; pressure 4.0MPa; space velocity 0.4h -1 The reaction of preparing diphenylamine by continuous condensation of aniline is carried out under the process conditions. When the conversion rate of aniline is less than 15% (mol), the catalyst is regarded as deactivated, and the production is shut down according to the shutdown plan to prepare for catalyst regeneration.

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Abstract

The invention relates to a catalyst regeneration method used for preparing diphenylamine by aniline consecutive condensation. The method is a method of coke burning regeneration of nitrogen including oxygen in an adoption device, and comprises the steps of purging the complete system with nitrogen to remove reaction mixture, reducing the temperature of the system and replacing the oxygen gas by nitrogen, wherein, the regenerated temperature and the oxygen content are strictly controlled by adopting a method of multiple step burning regeneration, the operation is simple, the regenerating time is short, and the physicochemical property and the activity index of the regenerated catalyst are basically identical to the fresh catalyst.

Description

technical field [0001] The invention relates to a regeneration method of a catalyst for preparing diphenylamine by continuous condensation of aniline, in particular to a regeneration method of a catalyst containing Hβ zeolite and alumina. Background technique [0002] As we all know, diphenylamine has many uses. It can be used as antioxidant, dyeing accelerator and stabilizer of rubber, and is an intermediate of many chemical products. The traditional production method of preparing diphenylamine with aniline as raw material is gap kettle type, liquid phase catalytic synthesis method, because the method uses aluminum trichloride as catalyst, equipment corrosion is serious in production, environment is polluted, reaction selectivity is low, catalyst It is difficult to separate from the product, the unit consumption of raw materials is high, and the cost of the product is high. [0003] US44534348 and US3118944 patents describe that during the gas-phase preparation of diphenyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J38/14B01J38/20B01J29/70
Inventor 宋丽芝艾抚宾王海波勾连科
Owner CHINA PETROLEUM & CHEM CORP
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