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Treating method for vulcanized hydrogenation catalyst

A technology of hydrogenation catalyst and treatment method, which is applied in physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of loss of active components and decrease of catalyst activity, saving start-up time and improving processing time. Hydrogen activity, easy storage effect

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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  • Treating method for vulcanized hydrogenation catalyst
  • Treating method for vulcanized hydrogenation catalyst
  • Treating method for vulcanized hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation of embodiment 1 catalyst A

[0029] 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.

[0030] Put catalyst A into the reactor, directly raise the temperature to 350°C, introduce raw material oil, and start the hydrogenation reaction at constant temperature for 6 hours, and take samples for analysis after 24 hours of reaction. Reaction conditions: reaction temperature 350°C, reaction pressure 3.4MPa, hydrogen-to-oil ratio 360, volume space velocity 2.0, see Table 2 for th...

Embodiment 2

[0031] The preparation of embodiment 2 catalyst B

[0032] 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 300°C for 3 hours, cool down and take out the catalyst to obtain a vulcanized catalyst. Spray immersion 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.

[0033]Catalyst B was loaded into the reactor, and the start-up process and reaction conditions were the same as in Example 1, and its hydrodesulfurization activity was shown in Table 2.

Embodiment 3

[0034] The preparation of embodiment 3 catalyst C

[0035] Take 100g of catalyst III in oxidation state, feed hydrogen, heat up to 150°C and start to feed vulcanized oil, the vulcanized oil contains 5% (v%) of dimethyl disulfide, keep the temperature for 1 hour, then continue to heat up to 230°C for 3 hours. , after which the temperature was raised to 300°C for 3 hours to be vulcanized, and the temperature was lowered to take out the catalyst to obtain a sulfurized catalyst. Spray immersion with an aqueous solution of nickel citrate (5.0g / 100ml in terms of nickel), so that the introduced nickel citrate (in terms of nickel oxide) accounts for 1.5% of the weight of the sulfurized catalyst, and then treat it in air at 120°C After 12 hours, catalyst C was obtained.

[0036] Put catalyst C into the reactor, directly raise the temperature to 370°C, introduce raw material oil, and start the hydrogenation reaction at constant temperature for 6 hours, and take samples for analysis aft...

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Abstract

The invention discloses a treating 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; and carrying out heat treatment so as to allow a layer of a protective film to form on the surface of the vulcanized hydrogenation catalyst. The method provided by the invention can passivate the vulcanized catalyst, facilitates transportation, storage and filling of the catalyst, enables the catalyst to be directly used without activation during operation and can improve hydrogenation performance of the catalyst.

Description

technical field [0001] The invention relates to a treatment 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): B01J27/051B01J27/049B01J29/16C10G45/08C10G47/20
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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