Grading method of fluidized bed catalyst

A catalyst and ebullating bed technology, which is applied in the gradation field of ebullating bed catalysts, can solve the problems of limiting the depth of hydrogenation reaction and the catalyst structure can not be well matched, and achieve the effect of improving the utilization rate

Active Publication Date: 2020-09-22
CHINA PETROLEUM & CHEM CORP +1
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  • Description
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Problems solved by technology

However, the current heavy oil hydrogenation catalyst gradation method is often studied from the surface level, that is, the catalyst particle size, pore size and activity transition, and does not consi

Method used

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  • Grading method of fluidized bed catalyst
  • Grading method of fluidized bed catalyst
  • Grading method of fluidized bed catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0041] This example provides a catalyst gradation combination and the preparation process of the gradation catalyst. Catalyst grading scheme is adopted, the catalyst is loaded in the reactor, and the bed is filled with hydrogenation catalyst I, hydrogenation catalyst II and hydrogenation catalyst III from top to bottom.

[0042] The preparation method of hydrogenation catalyst Ⅰ is as follows: the carrier Ⅰ is made of MoO 3 , NiO active components were supersaturated impregnated to obtain a catalyst precursor, which was dried at 250°C for 4h, heated to 580°C at 5°C / min, and roasted at constant temperature for 4.5h to obtain the desired catalyst. The catalyst MoO 3 is 21.5%, NiO is 5.9%; the specific surface area is 100m 2 / g, the pore diameter is 17.8nm, the bulk density is 0.85g / mL, and the particle diameter is 3.0mm. Load the catalyst into the vulcanization reactor, introduce sulfurized oil into it, and wet the catalyst bed; then adjust the bed temperature to 170°C, and i...

Embodiment 2

[0046] With embodiment 1, only the preparation method of hydrogenation catalyst I, II and III is different, specifically:

[0047] The preparation method of hydrogenation catalyst Ⅰ is as follows: the carrier Ⅰ is made of MoO 3 , NiO active components were supersaturated impregnated to obtain a catalyst precursor, which was dried at 300°C for 5h, heated to 550°C at 4°C / min, and roasted at constant temperature for 4.5h to obtain the desired catalyst. The catalyst MoO 3 is 23.5%, NiO is 5.9%; the specific surface area is 130m 2 / g, the pore diameter is 21.5nm, the bulk density is 0.80g / mL, and the particle diameter is 2.5mm. Load the catalyst into the vulcanization reactor, introduce sulfurized oil into it, and wet the catalyst bed; then adjust the bed temperature to 170°C, and inject the vulcanizing agent; after the hydrogen sulfide penetrates the catalyst bed, the catalyst bed The bed temperature was raised to 260°C at a rate of 3°C / h and kept at a constant temperature for ...

Embodiment 3

[0051] Same as Example 2, only the preparation method of the hydrogenation catalyst III is different, specifically: the preparation method of the hydrogenation catalyst III is as follows: the carrier III is used to contain MoO 3 , NiO active components and lactose (the amount is 17% of the mass of the catalyst carrier) mixed solution saturated impregnation to obtain a catalyst precursor, the precursor was dried at 120 ° C for 1.5 h to obtain the desired catalyst. The catalyst MoO 3 is 11.9%, NiO is 3.0%; the specific surface area is 198m 2 / g, the pore diameter is 8.1nm, the bulk density is 0.67g / mL, and the particle diameter is 0.45mm. Load the catalyst into the vulcanization reactor, introduce sulfurized oil into it, and wet the catalyst bed; then adjust the bed temperature to 160°C, and inject the vulcanizing agent; after the hydrogen sulfide penetrates the catalyst bed, the catalyst bed The bed temperature was raised to 200°C at a rate of 15°C / h and kept constant for 4.5...

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Abstract

The invention discloses a fluidized bed catalyst grading method which comprises the following steps: heavy oil raw materials and hydrogen enter from the bottom of a reactor and are in contact with a hydrogenation catalyst bed layer for hydrogenation reaction, and a reaction product flows out from the top of the reactor; wherein the grading is filled with at least two stages of sulfurized hydrogenation catalysts; wherein from bottom to top in the material flow direction of the sulfurized hydrogenation catalysts at each stage, the average length of metal active phase crystals is gradually increased, the average number of lamellar crystal layers is gradually reduced, the content of active components is gradually reduced, the probable pore diameter is gradually reduced, the stacking density isgradually reduced, and the particle diameter is gradually reduced. The metal active phase is active metal sulfide. According to the method, the specific catalyst gradation is adopted, so that the active center of the catalyst can be effectively utilized, the coupling reaction performance of an active center structure and a reactant molecular structure is improved, the stability of hydrogenation reaction, such as demetalization, desulfurization and denitrification, of the whole system is greatly improved, and deep hydrogenation of heavy oil is facilitated.

Description

technical field [0001] The invention relates to a gradation method for ebullating bed catalysts. Background technique [0002] In the hydrotreating of heavy oil, catalysts are generally packed in grades, and the sequence is generally protective agent, demetallization, desulfurization and denitrogenation catalysts. The graded packing of the catalyst can not only increase the fouling capacity of the catalyst bed, but also significantly reduce the pressure drop of the catalyst bed. The use of catalyst graded loading technology can increase the metal capacity of the catalyst system at the same time, and because the upstream demetallization catalyst effectively exerts its demetallization function, it protects the hydrogenation activity of the downstream highly active desulfurizer or denitrification agent, so Catalyst graded loading technology can increase the hydrotreating capacity of residue hydrotreating catalysts for heavy raw materials. [0003] The reactions in the hydrotr...

Claims

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Application Information

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IPC IPC(8): C10G65/04
CPCC10G65/04C10G2300/107C10G2300/1074C10G2300/1077C10G2300/202C10G2300/205C10G2300/70
Inventor 吕振辉朱慧红金浩刘璐杨涛杨光
Owner CHINA PETROLEUM & CHEM CORP
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