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Startup sulfurization method for trickle bed class-II active center hydrogenation catalyst

A hydrogenation catalyst and active center technology, which is applied in the field of hydrogenation catalyst start-up vulcanization, can solve the problems of incomplete vulcanization wetting, increased processing costs, and insufficient vulcanization, etc., to achieve sufficient and thorough wetting, easy formation, and improved catalytic performance Effect

Active Publication Date: 2013-12-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Most of the existing hydrogenation technologies are in the form of trickle bed reactors. According to research, during the vulcanization process of the existing trickle bed reactors, the vulcanization and wetting in the hydrogenation catalyst are not complete, the vulcanization is not sufficient, or it is for Two vulcanizing agents are added to ensure vulcanization, which increases the processing cost and complicates the operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Put 100g of the metal salt catalyst with the second type of active center into a small reactor, and the airtightness is qualified. Adjust the hydrogen partial pressure to 6.0MPa and start to raise the temperature at 20°C / h. When it rises to 95°C, add sulfurized oil from the bottom of the reactor for wetting. . After the system is filled with vulcanized oil, enter the vulcanized oil from the top of the reactor instead, and carry out closed-circuit circulation of the device. The vulcanized oil is straight-run kerosene containing 2wt% carbon disulfide, and the conditions are that the volume ratio of hydrogen to oil is 350:1, and the volume space velocity is 2.0h -1 . Continue to raise the temperature to 180°C at 20°C / h, keep the temperature constant for 8 hours, and continue to raise the temperature at 20°C / h to 280°C at the end of the constant temperature, and keep the temperature constant for 3 hours. After the constant temperature is over, continue to raise the tempera...

Embodiment 2

[0042] Put 100g of the metal salt catalyst with the second type of active center into a small reactor, and the airtightness is qualified. Adjust the hydrogen partial pressure to 6.0MPa and start to raise the temperature at 20°C / h. When it rises to 140°C, add sulfurized oil from the bottom of the reactor for wetting. . After the system is filled with vulcanized oil, enter the vulcanized oil from the top of the reactor instead, and carry out closed-circuit circulation of the device. The vulcanized oil is straight-run kerosene containing 2wt% carbon disulfide, and the conditions are that the volume ratio of hydrogen to oil is 350:1, and the volume space velocity is 2.0h -1 . Continue to raise the temperature to 170°C at 20°C / h, keep the temperature constant for 8 hours, and continue to raise the temperature at 20°C / h to 280°C at the end of the constant temperature, and keep the temperature constant for 6 hours. After the constant temperature is over, continue to raise the temper...

Embodiment 3

[0044] Put 100g of the metal salt catalyst with the second type of active center into a small reactor, and the airtightness is qualified. Adjust the hydrogen partial pressure to 6.0MPa and start to raise the temperature at 20°C / h. When it rises to 140°C, add sulfurized oil from the bottom of the reactor for wetting. . After the system is filled with vulcanized oil, enter the vulcanized oil from the top of the reactor instead, and carry out closed-circuit circulation of the device. The vulcanized oil is straight-run kerosene containing 2wt% carbon disulfide, and the conditions are that the volume ratio of hydrogen to oil is 350:1, and the volume space velocity is 2.0h -1 . Continue to raise the temperature at 10°C / h to 170°C, keep the temperature for 8 hours, and continue to raise the temperature at 20°C / h to 270°C at the end of the constant temperature for 6 hours. After the constant temperature is over, continue to raise the temperature to 310°C at 20°C / h, and switch the raw...

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Abstract

The invention discloses a startup sulfurization method for a trickle bed class-II active center hydrogenation catalyst, which comprises the following steps: (1) preparing a class-II active center hydrogenation catalyst; (2) filling the class-II active center hydrogenation catalyst into a trickle bed reactor at normal temperature and normal pressure, introducing nitrogen to replace the air in a reaction system, sealing the nitrogen tightly, replacing the nitrogen with hydrogen, and sealing the hydrogen tightly; (3) regulating the temperature of a catalyst bed layer, introducing sulfurized oil from the bottom of the reactor, and wetting the class-II active center hydrogenation catalyst; (4) after the reactor is fully filled with sulfurized oil, introducing the sulfurized oil and hydrogen from the top of the reactor, forming closed-loop circulation in the reaction system, adding a sulfurizing agent into sulfurized oil gradually, and continuing to rise the temperature to complete sulfurization; and (5) after sulfurization is accomplished, introducing raw material oil from the top of the reactor. In the sulfurization method disclosed by the invention, the process is simple, the operation is convenient and quick, and the sulfurization effect is more ideal than the conventional method. Therefore, the method is more favorable for improving the number of class-II active center and consequently improving the activity of the catalyst.

Description

technical field [0001] The invention relates to a hydrogenation catalyst start-up vulcanization method, in particular to a hydrogenation catalyst start-up vulcanization method for a trickle bed type II active center. technical background [0002] Due to the slow growth of crude oil production and increasingly heavy quality, the demand for clean oil products in today's world is increasing, and the product quality requirements are becoming more and more stringent. The hydrogenation process of petroleum distillate is the main technology for producing clean oil products at present, and the preparation technology of hydrogenation catalyst is the key of hydrogenation technology. The active metal component of the prepared hydrogenation catalyst is generally in an oxidized state, and before the oxidized state catalyst is used in industry, its active metal must be converted into a sulfurized state to have a high catalytic activity. Therefore, the sulfidation of the catalyst has an i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10G49/24C10G45/00C10G47/00
Inventor 陈光高玉兰王继峰徐黎明李崇慧
Owner CHINA PETROLEUM & CHEM CORP
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