Startup method of sulfuration type hydrogenation catalyst

A hydrogenation catalyst and a sulfurized type technology are applied in the field of the start-up of sulfurized hydrogenation catalysts, which 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...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The preparation of embodiment 1 catalyst A

[0035] Get 100g oxidation state catalyst I, 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 A was obtained.

[0036] Put catalyst A into the reactor, keep the nitrogen pressure at 3.4MPa, directly raise the temperature to 120°C, introduce straight-run diesel oil, continue to raise the temperature to 300°C, keep the temperature for 6 hours, then cool down to 280°C, replace the nitrogen with hydrogen, and replace the raw materials at the same time Oil, the hydrogenation reaction starts after 24 ho...

Embodiment 2

[0037] The preparation of embodiment 2 catalyst B

[0038] 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.

[0039] The start-up and reaction conditions are the same as in Example 1, and the hydrodesulfurization activity is shown in Table 2.

Embodiment 3

[0040] The preparation of embodiment 3 catalyst C

[0041] 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.

[0042] Put catalyst C into the reactor, start the circulating compressor after the airtightness is qualified, raise the pressure to 4.0MPa with nitrogen, raise the temperature of the catalyst bed to 120°C, introduce coked kerosene (nitrogen content is 0.035wt%), and continue to raise the temperature to 300°C, keep the temperature constant for 6 hours, then cool down to 280°C, replace...

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Abstract

The invention discloses a startup method of a sulfuration type hydrogenation catalyst. The method comprises the following steps: the sulfuration type hydrogenation catalyst is impregnated by using an organic complex solution of a VIII-group metal; a heat treatment is carried out, such that a protection film is formed on the surface of the sulfuration type hydrogenation catalyst; startup oil is introduced under the existence of an inert gas, and a treatment is carried out; the inert gas is switched into hydrogen, and the pressure and temperature are regulated to reaction pressure and reaction temperature when the gas flow is stable; raw oil is fed, and the hydrogenation reaction is started. With the method provided by the invention, the sulfuration type hydrogenation catalyst can be passivated, such that catalyst transportation, storage and loading are convenient. Also, the hydrogenation performance of the catalyst can be improved.

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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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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