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Preparation method for granular hydrogenation catalyst

A hydrogenation catalyst and small particle technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of downstream reaction or equipment impact, increased catalyst consumption, high wear of spherical particles, etc. The preparation process is simple and easy, the anti-wear performance is strong, and the effect of reducing the impact is achieved.

Active Publication Date: 2013-10-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above methods can prepare low-wear small-particle catalysts or carriers, but special equipment is required for spheroidization, the preparation process is complicated, and the cost of the catalyst is increased. Moreover, the obtained spherical particles have high wear, increase catalyst consumption, and affect downstream reactions or equipment. bring adverse effects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0038] In the preparation process of the catalyst of the present invention, in the described acidic aluminum salt solution, Al 2 o 3 The concentration is 2-10g / 100mL; in the alkaline aluminate aqueous solution, Al 2 o 3 The concentration is 8-30g / 100mL.

[0039] Among the present invention, catalyst specific surface and pore structure adopt low-temperature liquid nitrogen adsorption method to measure; Phase adopts X-ray diffraction analysis; Acid index test method: get a certain amount of dry glue (with Al 2 o 3 Count) by mass ratio Al 2 o 3 : HNO 3 =1:0.2 After adding concentrated nitric acid with a mass concentration of 65%, the Al in the peptizable part 2 o 3 The percentage of total alumina is the acidity index; abrasion is measured by sieving.

Embodiment 1

[0042] 2L sodium metaaluminate aqueous solution (Al 2 o 3 Concentration is 15g / 100mL) and 3L aqueous solution of aluminum sulfate (Al 2 o 3 Concentration is 2g / 100mL) into the container at the high position, the flow meter connected to the bottom flows into the stainless steel container equipped with 6L clean water belt agitator and heating mantle, and heated to 40°C; add sodium metaaluminate solution to make the pH value rises to 9.8, stop adding sodium metaaluminate solution, and stabilize for 10 minutes; pass through aluminum sulfate solution, reduce the pH value to 3, and stabilize for 10 minutes; pass through sodium metaaluminate solution, make the pH value rise to 10. Repeat the swing 3 times. After the swing is over, stabilize for 10 minutes, add 250mLMoO 3 and NiO ammonia solution (MoO 3 15g / 100mL, NiO 3.0g / 100mL) was heated to 130°C and stabilized for 3 hours, the mother liquor was separated by filtration and washed. Dried at 140°C for 3 hours to obtain dry glue...

Embodiment 2

[0044] 2L sodium metaaluminate aqueous solution (Al 2 o 3 Concentration is 20g / 100mL) and 3L aqueous solution of aluminum sulfate (Al 2 o 3 Concentration is 8g / 100mL) respectively into the container at the high position, the flow meter connected to the bottom flows into the stainless steel container equipped with 6L clean water with stirrer and heating mantle, and heated to 55°C; add sodium metaaluminate solution to make the pH value rises to 10.8, stop adding sodium metaaluminate solution, and stabilize for 10 minutes; pass through aluminum sulfate solution, make the pH value drop to 3.5, and stabilize for 10 minutes; pass through sodium metaaluminate solution, make the pH value rise to 10.8. Repeat the swing 4 times. After the swing is over, after 10 minutes of stabilization, add 300mLMoO 3 and NiO ammonia solution (MoO 3 15.0g / 100mL, NiO 4.0g / 100mL) was heated to 160°C and stabilized for 4 hours, the mother liquor was separated by filtration and washed. Dried at 100°C...

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PUM

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Abstract

The invention discloses a preparation method for a granular hydrogenation catalyst. The method comprises the following steps of: preparing aluminum hydroxide colloid at a relatively low temperature by adopting pH value oscillation colloid formation, adding an ammonia solution containing Mo and Ni after the low-temperature colloid formation, stabilizing the solution for certain time at a high temperature, filtering, washing, drying, crushing the dried colloid powder into granules, and thus obtaining the granular hydrogenation catalyst by roasting. By the method, the granular hydrogenation catalyst with large aperture, large specific surface area, low abrasion and uniform active metal distribution can be prepared. The hydrogenation catalyst is particularly suitable to be used as a boiling bed residuum hydro-treating catalyst, and can reduce the diffusion limitation of macromolecular compounds such as colloid and bituminous matter and the like in the residuum in the catalyst; the hydrogenation reaction activity of the catalyst can be improved; the catalyst has strong abrasion resistance; the consumption of the catalyst is reduced; and meanwhile, the influence of the catalyst on the downstream reaction or equipment is also reduced.

Description

technical field [0001] The invention relates to a preparation method of a small-particle hydrogenation catalyst, which is particularly suitable for the preparation of a small-particle, low-wear hydrogenation catalyst in the fluidized bed hydrogenation treatment process of heavy oil and residual oil. technical background [0002] Most of the impurities such as sulfur and metals in crude oil are concentrated in the residual oil, and these impurities will pollute the downstream catalysts in the subsequent processing, so these impurities must be removed by hydrotreating first. [0003] Residue hydrotreating processes mainly include fixed bed, moving bed and ebullating bed. The fluidized bed hydrogenation process is one of the effective means for deep processing of heavy oil due to its strong adaptability to raw materials and flexible processing schemes. [0004] In the process of heavy oil ebullating bed hydroprocessing, raw oil and hydrogen flow upward through the catalyst bed...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/04
Inventor 刘喜来王刚隋宝宽刘文杰
Owner CHINA PETROLEUM & CHEM CORP
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