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On-line regeneration method of deactivated palladium catalyst in coal-to-ethylene glycol process

A coal-to-ethylene glycol and palladium catalyst technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve cumbersome process, long time-consuming and low cost and other problems, to achieve the effect of low activation temperature, low cost, and solve the problem of regeneration

Active Publication Date: 2016-06-15
贵州鑫醇科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] It can be seen that the above regeneration method either requires the introduction of organic matter and / or acid to fully contact the catalyst, or the treatment temperature needs to exceed 500°C, and the activation of the catalyst needs to be disassembled from the device for activation treatment, which is not environmentally friendly, and the process is cumbersome and time-consuming.
[0009] At present, there is no regeneration method after the deactivation of the palladium-containing catalyst used in the coal-to-ethylene glycol technology. Therefore, a regeneration method suitable for the deactivation of the palladium-containing catalyst used in the coal-to-ethylene glycol technology is developed, so that the entire regeneration process can It is carried out in the existing fixed-bed reactor, which can not only save the regeneration time, but also has low cost, which is of great significance for the development of coal-to-ethylene glycol technology

Method used

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  • On-line regeneration method of deactivated palladium catalyst in coal-to-ethylene glycol process
  • On-line regeneration method of deactivated palladium catalyst in coal-to-ethylene glycol process
  • On-line regeneration method of deactivated palladium catalyst in coal-to-ethylene glycol process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] exist figure 1 In the shown coal-to-ethylene glycol plant, the palladium catalysts in the dehydrogenation reactors 101 and 102 and the synthesis reactors 201 and 202 are simultaneously regenerated.

[0030] Before regeneration, close the reaction gas first, stop the operation of the coal-to-ethylene glycol unit, and feed N through the regeneration gas inlet of 110 2 , cool down to room temperature, purge the reactor and the regeneration pipeline, turn on the circulation compressor and the venting device, and control the venting volume at 10%. After 6h, the CO content in the circulating gas is 0.95%, and the gas replacement is completed. Gradually raise the temperature of 101 and 102 to 120°C, gradually raise the temperature of 201 and 202 to 150°C, pass water vapor from 110 to replace N 2 , the venting amount is controlled at 5%, after 3h, the water vapor content in the circulating gas is 70%, and the space velocity is 3000h -1 , Continuous reaction for 20h to remove ...

Embodiment 2

[0035] exist figure 1 In the coal-to-ethylene glycol unit shown, the palladium catalysts of the 101 and 102 dehydrogenation reactors were regenerated individually.

[0036] Refer to Example 1 for the gas circuit control and replacement process of the regeneration process. Before regeneration, turn off the reaction gas, stop the operation of the coal-to-ethylene glycol unit, and feed N 2 , cooled to room temperature, purged the reactor and regeneration pipeline, completed gas replacement after 3 hours, gradually heated 101 and 102 to 130 °C, and introduced water vapor to remove some organic and inorganic substances attached to the surface of the catalyst, and the space velocity was 1000h -1 , after continuous reaction for 12h, N was introduced 2 Replace the water vapor, and then heat up 101 and 102 to 300 ℃, the space velocity is 2000h -1 Constant temperature for 24h, dredging the pores of the carrier, after that, use O 2 to N 2 Replace and heat 101 and 102 to 250°C with ...

Embodiment 3

[0038] exist figure 1 In the coal-to-ethylene glycol unit shown, the palladium catalysts of the 201 and 202 synthesis reactors were individually regenerated.

[0039] Refer to Example 1 for the gas circuit control and replacement process of the regeneration process. Before regeneration, turn off the reaction gas, stop the operation of the coal-to-ethylene glycol unit, and feed N 2 , cooled to room temperature, purged the reactor and regeneration pipeline, completed gas replacement after 8 hours, gradually heated 201 and 202 to 150 °C, and introduced water vapor to remove some organic and inorganic substances attached to the surface of the catalyst. The space velocity is 3000h -1 , after continuous reaction for 20h, feed N 2 Replace water vapor, and then heat up 201 and 202 to 350 ° C, the space velocity is 4000h -1 Constant temperature for 30h, dredging the pores of the carrier, after that, use O 2 to N 2 Replace and heat 201 and 202 to 350°C with a space velocity of 250...

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Abstract

The invention discloses an online regeneration method of deactivated palladium catalyst in coal-to-ethylene glycol process. The whole regeneration process is carried out in the existing fixed-bed reactor, and water vapor is passed in at different temperatures to remove part of the organic matters attached to the surface of the catalyst. and inorganic matter, pass into N 2 To dredge the carrier channel, pass O 2 To remove the carbon deposit on the catalyst, and oxidize and disperse the agglomerated reduced palladium, and pass H 2 The active component is reduced and redispersed. After regeneration, the activity of the catalyst can be basically restored, and the performance is slightly lower than that of a fresh catalyst, which can continue to be used for half a year. The regeneration method adopted in the present invention does not need to unload the catalyst from the fixed bed. The method is simple, economical and easy to operate, and has great significance for the development of coal-to-ethylene glycol technology.

Description

technical field [0001] The invention relates to a regeneration method of a deactivated noble metal catalyst, in particular to an online regeneration method of a deactivated palladium catalyst in coal-to-ethylene glycol technology. Background technique [0002] Since the world's first 200,000-ton coal-to-ethylene glycol industrial demonstration plant was tested in Tongliao, Inner Mongolia, in December 2009, there has been an upsurge in the development and industrialization of coal-to-ethylene glycol technology at home and abroad. At present, my country has built And the proposed coal-to-ethylene glycol industrial plant exceeds 5 million tons. [0003] The coal-to-ethylene glycol technology is divided into two steps. The first step is carbon monoxide carbonylation coupling to synthesize oxalate. The second step is hydrogenation of oxalate to prepare ethylene glycol. , involving two catalytic reactions, respectively dehydrogenation and purification of carbon monoxide raw materi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/96C07C69/36C07C67/36
CPCY02P20/584
Inventor 姚元根周张锋乔路阳崔国静宋珊珊潘鹏斌林凌覃业燕
Owner 贵州鑫醇科技发展有限公司
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