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In-situ presulfurization method of hydrogenation catalyst

A hydrogenation catalyst and vulcanized oil technology, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve problems such as incomplete vulcanization wetting, increased processing costs, and insufficient vulcanization, etc., to achieve Wetting is sufficient and thorough, preventing local dry areas, and the effect of complete vulcanization reaction

Active Publication Date: 2013-01-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its main disadvantage is that the vulcanization and wetting in the hydrogenation catalyst may not be complete, the vulcanization is not sufficient, or two vulcanizing agents are added to ensure sufficient 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

[0038]In industrial application, the catalyst must first undergo industrial drying, and the time used for industrial drying is about 24 hours. This test uses a small reaction device, so this process is not required. 100g of catalyst was loaded into a small reactor, and the airtightness was qualified. The hydrogen partial pressure was adjusted to 6.0MPa and the temperature was raised at 20°C / h. When the temperature was raised to 140°C, vulcanized oil was added 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 220°C at 20°C / h, keep the temperature constant for 8 hours, and continue to raise th...

Embodiment 2

[0040] In industrial application, the catalyst must first undergo industrial drying, and the time used for industrial drying is about 24 hours. This test uses a small reaction device, so this process is not required. 100g of catalyst was loaded into a small reactor, and the airtightness was qualified. The hydrogen partial pressure was adjusted to 6.0MPa and the temperature was raised at 20°C / h. When the temperature was raised to 140°C, vulcanized oil was added 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 220°C at 20°C / h, keep the temperature constant for 8 hours, and continue to raise t...

Embodiment 3

[0042] In industrial application, the catalyst must first undergo industrial drying, and the time used for industrial drying is about 24 hours. This test uses a small reaction device, so this process is not required. 100g of catalyst was loaded into a small reactor, and the airtightness was qualified. The hydrogen partial pressure was adjusted to 6.0MPa and the temperature was raised at 20°C / h. When the temperature was raised to 140°C, vulcanized oil was added 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 20°C / h to 230°C, keep the temperature for 6 hours, and continue to raise the temper...

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PUM

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Abstract

The invention discloses an in-situ presulfurization method of a hydrogenation catalyst. The method comprises the following steps: in the wetting stage of the catalyst, introducing sulfurized oil and hydrogen gas from the bottom of a reactor; when the reactor is full of the sulfurized oil, introducing the sulfurized oil and the hydrogen gas from the top of the reactor for closed cycle; and fillinga vulcanizing agent into the sulfurized oil gradually to complete sulfurization. In the method provided by the invention, the mode of introducing the sulfurized oil from the bottom of the reactor into the reactor is adopted for the wetting process of the catalyst, thus the wetting of the catalyst is more sufficient and complete, and the dry area in a catalyst bed can be effectively prevented; andmeanwhile, as the catalyst is fully wetted, the condition that the catalyst in the oxidation state is reduced by hydrogen gas thus the sulfurization is difficult to perform can be effectively avoided. The sulfurization method provided by the invention is simple in process and is convenient to operate, and the sulfurization effect is better than that of the conventional method, thereby being favorable for improving the activity of the catalyst.

Description

technical field [0001] The invention relates to an in-device vulcanization start-up method of a hydrogenation catalyst, in particular to an in-device pre-sulfurization start-up method of an oxidized state hydrogenation catalyst. 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 in an oxidized state, and before the oxidized state catalyst is used in industry, its active metal needs to be converted into a sulfurized state to have high catalytic activity. Therefore, the sulfidation of the catalyst has ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10G45/08B01J37/20
Inventor 陈光高玉兰徐黎明李崇慧
Owner CHINA PETROLEUM & CHEM CORP
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