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Vulcanization method of hydrofining catalyst

A hydrogenation catalyst and catalyst technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., to achieve the effect of improving the activity of deep hydrodesulfurization

Active Publication Date: 2014-12-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the deficiencies of existing hydrogenation catalyst sulfidation methods, and provides a sulfidation method that is beneficial to the formation of Co-Mo-S or Mo-Ni-S active phases of diesel deep desulfurization catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In the medium-scale test device, the molybdenum-nickel type diesel deep hydrodesulfurization catalyst developed by Fushun Petrochemical Research Institute was used for sulfuration. The properties of the catalyst are shown in Table 1. As the vulcanized oil, ordinary second-line diesel is used as the vulcanized oil, and the properties of the vulcanized oil are shown in Table 2. Vulcanizing agent selects dimethyl disulfide for use.

[0029]After the airtightness of the device is qualified, the pressure of the device is raised to 6.0 MPa with nitrogen, the compressor is started to establish nitrogen circulation, and then the reaction temperature is raised to 150°C at 25°C / h. Start the raw material oil pump to inject sulfurized oil. After the catalyst bed is wetted, gradually increase the temperature of the catalyst bed to 230°C, discharge the system nitrogen, and release the pressure of the device to 1.0MPa. Then, introduce the concentration of hydrogen sulfide into the sys...

Embodiment 2

[0031] On the medium-scale test device, the same diesel deep hydrodesulfurization catalyst as in Example 1 was used for sulfidation. The vulcanized oil is selected from Table 2 vulcanized oil. Vulcanizing agent selects carbon disulfide for use.

[0032] After the airtightness of the device is qualified, the pressure of the device is raised to 6.0 MPa with nitrogen, the compressor is started to establish nitrogen circulation, and then the reaction temperature is raised to 150°C at 25°C / h. Start the raw material oil pump to inject sulfurized oil. After the catalyst bed is wetted, gradually increase the temperature of the catalyst bed to 280°C, discharge the system nitrogen, and release the pressure of the device to 1.0MPa. Then, introduce the concentration of hydrogen sulfide into the system through the circulating compressor At the same time, inject the vulcanizing agent carbon disulfide into the system, increase the pressure to 6.0MPa with hydrogen containing hydrogen sulfide...

Embodiment 3

[0034] On a medium-scale test device, the same diesel deep hydrodesulfurization catalyst as in Example 1 was used to carry out wet and dry combined vulcanization. The vulcanized oil is selected from Table 2 vulcanized oil. Vulcanizing agent selects dimethyl disulfide for use.

[0035] After the airtightness of the device is qualified, the pressure of the device is raised to 6.0MPa with nitrogen, the compressor is started to establish nitrogen circulation, and then the reaction temperature is raised to 175°C at 25°C / h. Start the raw material oil pump to inject sulfurized oil. After the catalyst bed is wetted, gradually increase the temperature of the catalyst bed to 250°C, discharge the system nitrogen, and release the pressure of the device to 1.0MPa. Then, introduce the concentration of hydrogen sulfide into the system through the circulating compressor At the same time, inject the vulcanizing agent dimethyl disulfide into the system, increase the pressure to 5.0MPa with hyd...

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Abstract

The invention discloses a vulcanization method of a hydrofining catalyst. The method comprises: first, under a nitrogen atmosphere, raising the catalyst bed temperature to 120-180DEG C, and starting injection of vulcanization startup oil; after complete moistening, raising the catalyst bed temperature to 230-260DEG C, using hydrogen sulfide-containing hydrogen to replace nitrogen in the reaction system, and beginning to injecting a vulcanizing agent into the reaction system; and when the purity of hydrogen in a circulation gas is greater than 75%, carrying out vulcanization according to a normal vulcanization process. According to the invention, the introduction of hydrogen sulfide and injection of the vulcanizing agent are carried out under a higher temperature, low temperature individual vulcanization of Co and / or Ni can be avoided, so that under a high temperature and in the presence of hydrogen sulfide, Mo and / or W, and Co and / or Ni can be vulcanized at the same time to form a high activity Mo(W)-Co(N)-S active phase. The method provided in the invention is in favor of improving the deep hydrodesulfurization activity of the catalyst.

Description

technical field [0001] The invention relates to a method for sulfiding a hydrorefining catalyst, in particular to a method for presulfurizing a diesel deep hydrorefining catalyst. Background technique [0002] With the improvement of people's awareness of environmental protection and the increasingly stringent environmental regulations, the production and use of clean vehicle fuels has increasingly become a development trend. Environmental regulations have very strict requirements on the content of impurities such as sulfides and aromatic compounds in gasoline and diesel for vehicles. In clean diesel production and diesel quality improvement technologies, hydrofining technology is still the main and most effective technical means. Hydrofining refers to the chemical process of hydrodesulfurization, hydrodenitrogenation, hydrodeoxygenation, and aromatics saturation under the conditions of certain hydrogen pressure, certain reaction temperature and the presence of hydrofining ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10G45/08B01J37/20
Inventor 柳伟刘继华李扬宋永一牛世坤李士才徐大海丁贺赵桂芳
Owner CHINA PETROLEUM & CHEM CORP
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