Regeneration method for catalyst used for methylation of toluene

A toluene methylation catalyst and methylation technology are applied in catalyst regeneration/reactivation, physical/chemical process catalyst, molecular sieve catalyst, etc., and can solve the problems of complex equipment, cumbersome regeneration steps, poor recovery of catalyst activity, etc. Achieving good technical effect and good effect of active recovery

Active Publication Date: 2014-05-07
CHINA PETROLEUM & CHEM CORP +1
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AI-Extracted Technical Summary

Problems solved by technology

[0013] The technical problem to be solved by the present invention is that the regeneration steps of the toluene methylation catalyst in the prior art are cu...
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Abstract

The invention relates to a regeneration method for a catalyst used for methylation of toluene, and mainly solves the problems in the prior art that the regeneration steps of the methylation of toluene are cumbersome, equipment is complex, and catalyst activity is not properly regenerated. According to the invention, material stopping, separation, replacement, oxygen supplying, and other steps are carried out along with the adjustment of temperature and pressure of a reactor; the temperature of a catalyst bed is finally controlled to the constant value of 480-520 DEG C, and the oxygen content of the system reaches 0.45-0.55% by volume; the condition is kept for 1.0-10.0 h before the reaction stops gradually. According to the technical scheme of the regeneration method, the problems in the prior art can be excellently solved, and the method can be applied to the industrial production of mixed xylenes.

Application Domain

Molecular sieve catalystsCatalyst regeneration/reactivation +3

Technology Topic

ChemistryProcess engineering +3

Image

  • Regeneration method for catalyst used for methylation of toluene
  • Regeneration method for catalyst used for methylation of toluene
  • Regeneration method for catalyst used for methylation of toluene

Examples

  • Experimental program(7)
  • Comparison scheme(2)

Example Embodiment

[0034] [Example 1]
[0035] The deactivated JSM-03 catalyst was used for the regeneration test. The JSM-03 catalyst includes the following components in weight percentage: 69.27% ​​hydrogen type ZSM-5 molecular sieve with a silicon to aluminum ratio of 280, 30.68% Al 2 O 3 , 0.05% La 2 O 3.
[0036] The regeneration process is: stop feeding methylating reagents and toluene raw materials, and circulate hydrogen for 5 hours under the conditions of constant reaction temperature and pressure; gradually unload the system pressure to normal pressure and drop the temperature below 100°C; stop introducing hydrogen , Disconnect the liquid-phase feed system and product separation system to isolate the reactor system from the liquid-phase feed system and product separation system; replace the reaction system with nitrogen, and purge the system with nitrogen to make the total hydrogen and hydrocarbons in the system The concentration is less than 0.2% by volume; at the same time, raise the temperature of the reactor so that the catalyst bed temperature is 300°C, and adjust the system pressure to 0.3MPa; pass in air and observe the temperature rise of the catalyst bed. Once there is a temperature rise, immediately reduce the amount of injected air And reduce the temperature of the reaction system, wait for the temperature to stabilize, and then slowly pass in air, control the maximum bed temperature not to exceed 480℃, and the oxygen content in the system not to exceed 0.5% by volume; make the catalyst bed temperature constant at 480℃, increase air injection The oxygen content in the system reaches 0.5% by volume. After maintaining for 2 hours, the air is stopped, the system is gradually unloaded to normal pressure, the temperature drops to room temperature, and the regeneration process is ended.
[0037]

Example Embodiment

[0038] [Example 2]
[0039] The deactivated JSM-03 catalyst was used for the regeneration test.
[0040] The regeneration process is: stop feeding methylating reagents and toluene raw materials, and circulate water vapor for 3 hours under the conditions of constant reaction temperature and pressure; gradually unload the system pressure to normal pressure, and the temperature drops below 100°C; stop introducing water Steam shuts off the liquid-phase feed system and product separation system to isolate the reactor system from the liquid-phase feed system and product separation system; replace the reaction system with nitrogen and purge the system with nitrogen to make the hydrogen and hydrocarbons in the system separate The total concentration is less than 0.2% by volume; at the same time, raise the temperature of the reactor so that the temperature of the catalyst bed is 100℃, and adjust the system pressure to 1.0MPa; let in air and observe the temperature rise of the catalyst bed, once there is a temperature rise, immediately reduce the injected air The temperature of the reaction system is reduced, and the air is slowly introduced after the temperature is stable. The maximum temperature of the bed does not exceed 510℃, and the oxygen content in the system does not exceed 0.2% by volume; the temperature of the catalyst bed is kept constant at 510℃, and the air is increased The amount of injection is such that the oxygen content in the system reaches 0.45% by volume. After maintaining for 4 hours, the air is stopped, the system is gradually unloaded to normal pressure, and the temperature is lowered to room temperature to end the regeneration process.
[0041]

Example Embodiment

[0042] [Example 3]
[0043] The deactivated JSM-03 catalyst was used for the regeneration test.
[0044] The regeneration process is as follows: stop feeding methylating reagent and toluene raw materials, and circulate nitrogen for 2 hours under the condition of constant reaction temperature and pressure; gradually unload the system pressure to normal pressure, and drop the temperature below 100°C; stop introducing nitrogen , Disconnect the liquid-phase feed system and product separation system to isolate the reactor system from the liquid-phase feed system and product separation system; replace the reaction system with nitrogen, and purge the system with nitrogen to make the total hydrogen and hydrocarbons in the system The concentration is less than 0.2% by volume; at the same time, raise the temperature of the reactor to make the catalyst bed temperature 250℃, and adjust the system pressure to 0.6MPa; let air in, observe the temperature rise of the catalyst bed, once there is a temperature rise, immediately reduce the amount of air injected And lower the temperature of the reaction system, wait for the temperature to stabilize, and then slowly pass in air, control the maximum bed temperature not to exceed 490℃, and the oxygen content in the system not to exceed 0.1% by volume; make the catalyst bed temperature constant at 490℃, increase air injection The oxygen content in the system reaches 0.55% by volume. After maintaining for 1 hour, the air is stopped, the system is gradually unloaded to normal pressure, the temperature drops to room temperature, and the regeneration process is ended.
[0045]

PUM

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Classification and recommendation of technical efficacy words

  • Good technical effect
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