Hydrogenation catalyst start-up sulfidation method

A hydrogenation catalyst and sulfurized oil technology, which is applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc. Simple process and the effect of reducing consumption

Active Publication Date: 2022-08-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are a large number of light distillate oil hydrogenation units in China, including reforming pre-hydrogenation units, gasoline selective hydrodesulfurization units and jet fuel hydrogenation units. It is difficult for the system and heating furnace to meet the final sulfurization temperature of the new hydrogenation catalyst above 320°C

Method used

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  • Hydrogenation catalyst start-up sulfidation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] The fixed-bed reactor is filled with a hydrogenation catalyst, followed by nitrogen gas tightness, catalyst drying, introduction of hydrogen replacement, and hydrogen gas tightness. After the hydrogen gas tightness is qualified, the circulating hydrogen compressor is turned on to establish a full hydrogen circulation, and the hydrogen partial pressure is 1.6MPa. When the temperature of the catalyst bed in the reactor was raised to 150 °C, the starting sulfide oil was introduced to wet the catalyst bed, and the volumetric space velocity was 3.0 h. -1 , The high-pressure separator throws out the dirty oil until the oil is freed from solid mechanical impurities to establish a closed-circuit vulcanization cycle. The temperature of the catalyst bed was raised to 175°C at 15°C / h, and the vulcanizing agent was injected (based on the total circulating vulcanized oil in operation, the amount of the vulcanizing agent was 1% by weight) and detected H 2 S concentration. The hydro...

Embodiment 2

[0073] The hydrogenation catalyst is sulfidized according to the method of Example 1, and the difference is that the sulfidation temperature rise program is: to be heated to 230° C. at 15° C. / h (the first temperature rise stage, H 2 The S concentration is 0.1-0.3 vol%), and then constant temperature at 230°C for 6 hours (the first constant temperature stage, H 2The S concentration is 0.3-0.5% by volume), after the first constant temperature stage, 10% by volume of liquefied gas is introduced into the hydrogen mixing point, and the temperature is raised to 300 °C at 15 °C / h (the second heating stage, H 2 The S concentration is 0.5-1.0 vol%), and then constant temperature at 300°C for 8 hours (the second constant temperature stage, H 2 The S concentration is 1.0 to 1.5% by volume), and the vulcanization is completed. Then, according to the conditions of Example 1, the kerosene extracted from the constant line was introduced to carry out the hydrogenation reaction. After 48 hour...

Embodiment 3

[0075] The hydrogenation catalyst is sulfidized according to the method of Example 1, and the difference is that the sulfidation temperature rise program is: to be heated to 230° C. at 15° C. / h (the first temperature rise stage, H 2 The S concentration is 0.1-0.3 vol%), and then constant temperature at 230°C for 6 hours (the first constant temperature stage, H 2 The S concentration is 0.3-0.5% by volume), after the first constant temperature stage, 15% by volume of liquefied gas is introduced into the hydrogen mixing point, and the temperature is raised to 300 °C at 15 °C / h (the second heating stage, H 2 The S concentration is 0.5-1.0 vol%), and then constant temperature at 300°C for 8 hours (the second constant temperature stage, H 2 The S concentration is 1.0 to 1.5% by volume), and the vulcanization is completed. Then, according to the conditions of Example 1, the kerosene extracted from the constant line was introduced to carry out the hydrogenation reaction. After 48 hou...

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Abstract

The present disclosure relates to a method for starting sulfidation of a hydrogenation catalyst. The method comprises the following steps: a. introducing hydrogen into a fixed-bed reactor filled with a hydrogenation catalyst to establish a hydrogen cycle; b. hydrogenating the hydrogenation catalyst in the reactor The temperature of the catalyst bed is raised to 110-175°C, and then the start-up sulfide oil is introduced to wet the hydrogenation catalyst bed, and a closed-circuit cycle of the start-up sulfidation is established; c. Introduce a sulfidizing agent into the reactor, and increase the temperature according to the sulfidation. The hydrogenation catalyst is sulfided according to the program, and liquefied gas is introduced into the reactor in the heating stage of the sulfide temperature increase program. Based on the total circulating amount of the hydrogen, the amount of the liquefied gas is 5~ 20% by volume. The method can achieve a higher final sulfidation temperature of the hydrogenation catalyst under the condition that the heating capacity of the existing equipment in the refinery is limited, and at the same time, the energy consumption can be significantly reduced.

Description

technical field [0001] The present disclosure relates to a hydrogenation catalyst start-up sulfidation method. Background technique [0002] With the deterioration of crude oil resources around the world and the increasingly strict environmental regulations, it is necessary to produce a large number of high-quality clean fuels under harsh conditions. The environmental protection properties of the oil can be well improved by the hydrotreating of the oil, so that it is more optimized for the environment. Therefore, the fixed bed hydrotreating technology has been widely used. Fixed bed hydrotreating catalysts are generally oxidized catalysts, and their active metals (usually cobalt, molybdenum, nickel, and tungsten) are sold as commercial products in oxidized state. The metal is converted to the corresponding sulfided metal to achieve good catalyst activity. [0003] The fixed bed hydrogenation catalyst usually adopts the in-vessel pre-sulfiding technology, which is divided i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J37/20
CPCB01J37/20
Inventor 张锐习远兵丁石刘锋
Owner CHINA PETROLEUM & CHEM CORP
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