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Operating method for vulcanized hydrogenation catalyst

A hydrogenation catalyst, a vulcanization-type technology, which is applied in the field of start-up of a vulcanization-type hydrogenation catalyst, can solve the problems of loss of active components and decrease in catalyst activity, and achieve the effects of saving start-up time, improving hydrogenation activity, and being environmentally friendly

Active Publication Date: 2015-05-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst does not need to be activated when it is started, and can be used directly, but this method prevents part of the active metal phase from being completely converted into a highly active active phase, and part of the active components will be lost, resulting in a decrease in the activity of the catalyst.

Method used

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  • Operating method for vulcanized hydrogenation catalyst
  • Operating method for vulcanized hydrogenation catalyst
  • Operating method for vulcanized hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The preparation of embodiment 1 catalyst A

[0034] Get 100g oxidation state catalyst I, pass into the mixed gas of hydrogen and hydrogen sulfide, H 2 :H 2S=4:1, heat up to 300°C for 6 hours of vulcanization, cool down and take out the catalyst to obtain a vulcanized catalyst. Spray and immerse with an aqueous solution of nickel citrate (2.5g / 100ml in terms of nickel), so that the introduced nickel citrate (in terms of nickel oxide) accounts for 0.5% of the weight of the sulfurized catalyst, and then treat it at 150°C under nitrogen protection After 6 hours, catalyst A was obtained.

[0035] Put the catalyst A into the reactor, keep the nitrogen pressure at 3.4MPa, directly raise the temperature to 300°C, keep the temperature for 6 hours and then cool down to 280°C, replace the nitrogen with hydrogen, and introduce the raw material oil at the same time, start the hydrogenation reaction after 24 hours at the constant temperature, the reaction Samples were taken for an...

Embodiment 2

[0036] The preparation of embodiment 2 catalyst B

[0037] Take 100g of oxidation state catalyst II, pass through hydrogen, raise the temperature to 120°C and start to feed vulcanized oil, which contains CS 2 5% (v%), after constant temperature for 1 hour, continue to heat up to 230°C for 3 hours, then heat up to 320°C for 3 hours, cool down and take out the catalyst to obtain a vulcanized catalyst. Spray and immerse with an aqueous solution of cobalt citrate (concentration calculated as cobalt: 4.5g / 100ml), so that the introduced cobalt citrate (calculated as cobalt oxide) accounts for 1% of the weight of the sulfurized catalyst, and then treat it under air at 120°C for 12 hours, the catalyst B was obtained.

[0038] The start-up and reaction conditions are the same as in Example 1, and the hydrodesulfurization activity is shown in Table 2.

Embodiment 3

[0039] The preparation of embodiment 3 catalyst C

[0040] Get 100g oxidation state catalyst III, pass into the mixed gas of hydrogen and hydrogen sulfide, H 2 :H 2 S=4:1, heat up to 300°C for 6 hours of vulcanization, cool down and take out the catalyst to obtain a vulcanized catalyst. Spray and immerse with an aqueous solution of nickel citrate (2.5g / 100ml in terms of nickel), so that the introduced nickel citrate (in terms of nickel oxide) accounts for 0.5% of the weight of the sulfurized catalyst, and then treat it at 150°C under nitrogen protection After 6 hours, catalyst C was obtained.

[0041] Put the catalyst C into the reactor, start the circulating compressor after the airtightness is qualified, increase the pressure to 4.0MPa with nitrogen, raise the temperature of the catalyst bed to 300°C, keep the temperature constant for 6 hours, reduce the cracking section The inlet temperature of the inlet is up to 200°C, and then coking kerosene (nitrogen content is 0.035...

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Abstract

The invention discloses an operating method for a vulcanized hydrogenation catalyst. The method comprises the following steps: impregnating the vulcanized hydrogenation catalyst with an organic complex solution of a group-VIII metal; carrying out heat treatment so as to allow a layer of a protective film to form on the surface of the vulcanized hydrogenation catalyst; carrying out treatment in the presence of inert gas so as to allow the group-VIII metal to be inlaid in the defect of molybdenum disulfide or tungsten disulfide, thereby forming a high-activity hydrogenation active phase; and then carrying out switching into hydrogen, adjusting pressure and temperature to reaction pressure and reaction temperature after air current is steady, feeding raw oil and beginning a hydrogenation reaction. The method provided by the invention can passivate the vulcanized catalyst, facilitates transportation, storage and filling of the catalyst and can improve hydrogenation performance of the catalyst.

Description

technical field [0001] The invention relates to a start-up method of a sulfurized hydrogenation catalyst. Background technique [0002] Hydrogenation catalysts are generally supported by refractory porous non-chemical oxides, such as alumina, silica, titania, zirconia, etc., with Group VIB (Mo and / or W) and Group VIII metals (Co and / or Ni) is the active metal component. The hydrogenation catalyst is generally in an oxidized state before use, that is, the active metal exists in the form of an oxide, and the substance that actually plays an active role in actual use is a metal sulfide, so the active metal in the hydrogenation catalyst must be removed from the hydrogenation catalyst before use. The oxides are converted to sulfides. [0003] The vulcanization of hydrogenation catalysts is divided into internal pre-sulfurization and external pre-sulfurization. The in-vessel pre-sulfurization is carried out in the reactor, which not only increases the production cost, but also ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G49/24C10G47/00C10G45/00B01J27/051B01J27/049B01J29/16
Inventor 徐黎明高玉兰彭绍忠吕振辉张学辉孙海
Owner CHINA PETROLEUM & CHEM CORP
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