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Method for regenerating deactivated palladium catalyst on line in process of preparing ethylene glycol through coal

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

Active Publication Date: 2014-12-10
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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  • Method for regenerating deactivated palladium catalyst on line in process of preparing ethylene glycol through coal
  • Method for regenerating deactivated palladium catalyst on line in process of preparing ethylene glycol through coal
  • Method for regenerating deactivated palladium catalyst on line in process of preparing ethylene glycol through coal

Examples

Experimental program
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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 in dehydrogenation reactors 101 and 102 are regenerated separately.

[0036] Refer to Example 1 for the gas path control and replacement process of the regeneration process. Before regeneration, first turn off the reaction gas, stop the operation of the coal-to-ethylene glycol unit, and inject N 2 , cool down to room temperature, purge the reactor and the regeneration pipeline, and complete the gas replacement after 3 hours, gradually raise the temperature of 101 and 102 to 130°C, pass in water vapor to remove some organic and inorganic substances attached to the catalyst surface, and the space velocity is 1000h -1 , after continuous reaction for 12h, N 2 Replace the water vapor, then raise the temperature of 101 and 102 to 300°C, and the space velocity is 2000h -1 Constant temperature for 24h, dredge the carrier channel, after that, use O 2 to N 2 Carry out replacement, and raise th...

Embodiment 3

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

[0039] Refer to Example 1 for the gas path control and replacement process of the regeneration process. Before regeneration, first turn off the reaction gas, stop the operation of the coal-to-ethylene glycol unit, and inject N 2 , cool down to room temperature, purge the reactor and the regeneration pipeline, complete the gas replacement after 8 hours, gradually raise the temperature of 201 and 202 to 150°C, pass in water vapor to remove some organic and inorganic substances attached to the surface of the catalyst, and the space velocity is 3000h -1 , after continuous reaction for 20h, N 2 Replace the water vapor, then raise the temperature of 201 and 202 to 350°C, and the space velocity is 4000h -1 Constant temperature for 30h, dredge the carrier channel, after that, use O 2 to N 2 Carry out replacement, and raise the t...

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Abstract

The invention discloses a method for regenerating a deactivated palladium catalyst on line in process of preparing ethylene glycol through coal. The whole regeneration process is performed in a conventional fixed bed reactor. The process comprises the following steps: respectively introducing water vapor to remove partial organic matters and inorganic matters attached to the surface of the catalyst at different temperatures, introducing N2 to dredge a carrier pore channel, introducing O2 to remove carbon deposit on the catalyst, oxidizing and dispersing the aggregated palladium in a reduced state, introducing H2 to reduce and re-disperse active ingredients, and regenerating the catalyst so as to basically restore the activity of the catalyst, wherein the performance of the catalyst is slightly lower than that of a fresh catalyst, and the catalyst can be continuously used for half a year. According to the regeneration method adopted by the invention, the catalyst does not need to be discharged out of the fixed bed, and the method is simple, economical and easy to operate and has significance in developing a technology of producing ethylene glycol through coal.

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 Applications(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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