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Cryogenic passivation pretreatment process for nickel-based catalyst

A nickel-based catalyst and pretreatment technology, applied in catalyst activation/preparation, physical/chemical process catalyst, chemical/physical process, etc., can solve problems such as large equipment investment, and achieve high safety performance, easy activation, and process control conditions mild effect

Inactive Publication Date: 2016-01-13
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] For the pre-reduction technology outside the device, only preliminary research has been carried out in China, and there are still many difficulties in realizing industrialization, and these pre-reduction methods need to establish special devices, and the investment in equipment is relatively large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take QAH-01 for testing. Using hydrogen for external reduction, the reduction temperature is 450°C, and the reduction time is 10 hours. The active component is converted from nickel oxide to simple nickel. The hydrogen is recycled, and the amount of hydrogen added is 120% of the theoretical reduction hydrogen. After the reduction, when the catalyst bed temperature drops below 300°C, stop feeding hydrogen, and feed liquid carbon dioxide into the reactor to lower the temperature of the reduced catalyst to 40°C, and the liquid carbon dioxide liquid space velocity is 0.5h -1 , and after 2 hours of passivation treatment, stop adding liquid carbon dioxide, use 100h -1 Air at normal temperature blows away the liquid carbon dioxide in the system, and when the system outlet material does not contain liquid carbon dioxide, the catalyst passivation ends.

[0030] Among them, the pressure of the liquid carbon dioxide used is 5.28kg / cm 2 , the temperature of liquid carbon dioxide ...

Embodiment 2

[0032] Take Z502 for experiment. Using hydrogen for external reduction, the reduction temperature is 380°C, and the reduction time is 12 hours. The active component is converted from nickel oxide to simple nickel. The hydrogen is recycled, and the amount of hydrogen added is 110% of the theoretical reduction hydrogen. After the reduction, when the catalyst bed temperature drops below 300°C, stop feeding hydrogen, and feed liquid carbon dioxide into the reactor to lower the temperature of the reduced catalyst to 30°C, and the liquid carbon dioxide liquid space velocity is 2h -1 , and after 2.5 hours of passivation treatment, stop adding liquid carbon dioxide, use 100h -1 The air blows away the liquid carbon dioxide in the system, and when the system outlet material does not contain liquid carbon dioxide, the catalyst passivation ends.

[0033] Among them, the pressure of the liquid carbon dioxide used is 50kg / cm 2 , the temperature of liquid carbon dioxide is 15°C.

Embodiment 3

[0035] Take Z501 for experiment. Using hydrogen for external reduction, the reduction temperature is 450°C, and the reduction time is 6 hours. The active component is converted from nickel oxide to simple nickel. The hydrogen is recycled, and the amount of hydrogen added is 150% of the theoretical reduction hydrogen. After the reduction, when the catalyst bed temperature drops below 300°C, stop feeding hydrogen, feed liquid carbon dioxide into the reactor to lower the temperature of the reduced catalyst to 10°C, and the liquid carbon dioxide liquid space velocity is 2h -1 , and after 2.5 hours of passivation treatment, stop adding liquid carbon dioxide, use 50h -1 The air blows away the liquid carbon dioxide in the system, and when the system outlet material does not contain liquid carbon dioxide, the catalyst passivation ends.

[0036] Among them, the pressure of the liquid carbon dioxide used is 5.28kg / cm 2 , the temperature of liquid carbon dioxide is -56.6°C.

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PUM

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Abstract

The invention relates to a cryogenic passivation pretreatment process for a nickel-based catalyst. The process comprises the following steps: subjecting the nickel-based catalyst to ex-situ reduction treatment by using a reducing agent to allow an active component in the nickel-based catalyst to be converted into elementary nickel from nickel oxide; when the temperature of a catalyst bed is lowered to below 300 DEG C, stopping introduction of the reducing agent, then introducing liquid carbon dioxide into a reactor, cooling the reduced catalyst and carrying out passivation treatment for 2 to 3 hours, then stopping introduction of the liquid carbon dioxide, blowing the liquid carbon dioxide in the system away by using room-temperature air; and when an outlet material does not contain the liquid carbon dioxide, completing passivation of the nickel-based catalyst. The cryogenic passivation pretreatment process for the nickel-based catalyst provided by the invention has the advantages of mild control conditions, high degree of reduction and uniform reduction; the reduced catalyst can stably exist in air and is not affected by passivation pretreatment in activity and stability at the same time; when in use, the catalyst is easy to activate, has short activation time and high shift activity, is convenient for transportation and storage, and significantly reduces working time of enterprises and adverse conditions brought by reduction of the catalyst in a device.

Description

technical field [0001] The invention relates to a catalyst reduction technology, in particular to a nickel-based catalyst cryogenic passivation pretreatment process. Background technique [0002] Nickel-based catalysts are widely used in industry, such as hydrocarbon steam reforming, methanation, hydrogenation, etc. Experiments and industrial applications have proved that only the reduction treatment of nickel-based catalysts can convert the active components in the oxidized state into elemental nickel. In order to make it have hydrogenation and dehydrogenation activity, the reduction effect of the nickel-based catalyst directly affects the performance of the catalyst. [0003] Nickel-based catalysts often adopt external pre-reduction treatment or internal reduction treatment technology, and the internal reduction treatment technology has obvious shortcomings, (a) requires special pre-reduction equipment and instruments; (b) the reduction time is long, affecting normal Star...

Claims

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Application Information

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IPC IPC(8): B01J37/18
Inventor 王昊白志敏薛红霞姜建波余汉涛赵庆鲁齐焕东宋晓军
Owner CHINA PETROLEUM & CHEM CORP