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Pre-treatment method of nickel hydrogenation catalyst

A technology for hydrogenation catalysts and nickel-based catalysts, applied in chemical instruments and methods, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, etc. Bed hot spots, catalyst activity and selectivity decline, etc., to achieve excellent hydrogenation activity and selectivity, easy control of bed temperature rise, and excellent hydrogenation stability

Active Publication Date: 2010-09-08
PETROCHINA CO LTD
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AI Technical Summary

Problems solved by technology

During the reduction process of nickel oxide, highly dispersed metallic nickel is easy to aggregate above 400°C, which reduces the dispersion of active components
In the reduction process mentioned in the above two patents, the catalyst needs to be treated in the presence of hydrogen at a temperature above 400°C for 10 to 15 hours, resulting in the catalyst needing to withstand high temperature for a long time, and the reduced active component nickel metal is easily exposed to high temperature for a long time. Promoting the growth of nickel grains, reducing the number and dispersion of active sites, resulting in a decrease in catalyst activity and selectivity
Moreover, the catalysts mentioned in the above two patents are provided to the device in a sulfurized state. At the beginning of the catalyst’s use process, the sulfur in the catalyst is easily washed and lost by the start-up oil, which reduces the sulfuration efficiency. The initial reaction activity is high and the heat release is concentrated. prone to bed hot spots

Method used

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  • Pre-treatment method of nickel hydrogenation catalyst
  • Pre-treatment method of nickel hydrogenation catalyst
  • Pre-treatment method of nickel hydrogenation catalyst

Examples

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preparation example Construction

[0034] Preparation of Catalyst 1:

[0035] Add 140L of water and 5L of nitric acid (content 60%) to 300kg of pseudoboehmite alumina powder, knead and extrude into strips, dry at 120°C in the air, and roast at 900-1100°C to obtain Al 2 o 3 carrier. Add nickel nitrate to 200L-300L water, stir and dissolve, adjust the pH value to 4, then impregnate on 100kg carrier, age for 12 hours, dry at 120°C, and roast at 400°C for 4 hours to prepare the catalyst. The physical and chemical properties of the catalysts obtained are shown in Table 2.

[0036] Preparation of Catalyst 2:

[0037] Add 140L of water, 5L of nitric acid (content 60%), silica sol (containing 40% silicon dioxide) to 300kg of pseudo-boehmite alumina powder, knead and extrude into strips, dry in the air at 120°C, 900~ Calcined at 1100°C to obtain corresponding modified Al 2 o 3 carrier. Add nickel nitrate to 200L-300L water, stir and dissolve, adjust the pH value to 4, then impregnate on 100kg carrier, age for 12 ...

Embodiment 1

[0044] Put the catalyst 1 into the fixed bed reactor, under the pressure of 0.4MPa, the volume ratio of hydrogen to the catalyst is 500Nm 3 / m 3 / h, raise the temperature of the bed layer to 240°C at a rate of 50°C / h and maintain it for 5h, then raise the temperature to 340°C at a rate of 10°C / h, maintain it for 10h, and then raise the temperature to 400°C at a rate of 15°C / h , maintained for 5 hours; then lowered the temperature to 35°C, fed a mixture of nitrogen and air, the initial partial pressure of oxygen was 5%, and gradually increased the partial pressure of oxygen under the condition that the temperature rise of the reactor did not exceed 5°C until the partial pressure of oxygen was 20%, maintained for 5 hours, a pre-reduced / oxidized catalyst was obtained.

[0045] Put the catalyst into an adiabatic bed reactor, raise the temperature of the bed to 150°C at a rate of 50°C / h under the hydrogen pressure of 2.0MPa and maintain it for 10h, then cool down the catalyst bed ...

Embodiment 2

[0047] Put the catalyst 2 into the adiabatic bed hydrogenation reaction device, under the pressure of 0.8MPa, feed the helium-hydrogen mixed gas with the hydrogen content of 10%, and the volume ratio of the reducing gas to the catalyst is 1000Nm 3 / m 3 / h, raise the temperature of the bed layer to 250°C at a rate of 40°C / h and maintain it for 4h, then raise the temperature to 350°C at a rate of 8°C / h, maintain it for 8h, and then raise the temperature to 390°C at a rate of 12°C / h , maintained for 4 hours; then cooled to 25°C, under the hydrogen pressure of 2.5MPa, naphtha with a sulfur content of 450ug / g and an olefin content of 1.2% passed through the catalyst bed at a space velocity of 12 hours -1 , The passivation time is 3 hours.

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Abstract

The invention relates to a pre-treatment method of a nickel hydrogenation catalyst, which mainly comprises two steps that: (1) when reducing gas exists, the catalyst is reduced on a fixed bed reactor or a converter through a segmentation method, the volume ratio of the reducing gas to the catalyst is 500 to 1000Nm3 / m3 / h, and the process conditions are as follows: the pressure is 0.1 to 0.8MPa, the temperature goes up to 230 to 250 DEG C at the temperature rise speed of 15 to 50DEG C / h and is maintained for 3 to 5h, and then goes up to 390 to 400DEG C at the temperature rise speed of 10 to 20DEG C / h and is maintained for 4 to 5h, and the reduction is over; and (2) catalyst passivation: the hydrogen pressure is 2.0 to 3.0MPa, the temperature of a catalyst bed layer is 20 to 30DEG C, the passivator airspeed is 5 to 20h-1, and the passivator and the catalyst contact for 3 to 5h; and the passivator is an oil product which contains olefin, the olefin mass content is 0.1 to 40 percent, and the sulfur content is 0 to 500mu g / g.

Description

technical field [0001] The present invention relates to a pretreatment method of a hydrogenation catalyst, in particular to a pretreatment method of a nickel-based hydrogenation catalyst, in particular to a pretreatment method of a nickel-based catalyst for selective hydrogenation of diolefins in full-run pyrolysis gasoline into monoolefins Approach. Background technique [0002] In the process of selective hydrogenation of dienes, especially in the process of selective hydrogenation of pyrolysis gasoline, the catalysts currently used in industry are mainly Pd-based or Ni-based catalysts. Although the traditional palladium catalyst is widely used in industrial devices, because the palladium content in the catalyst is only a few per thousand, and it is located on the surface of the catalyst, it is sensitive to impurities such as arsenic and water. And the differences in cracking methods have caused some manufacturers to deteriorate the cracking gasoline raw materials, increa...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J23/78B01J23/83B01J23/85B01J37/18C07C5/05
Inventor 钱颖梁顺琴颉伟秦鹏吴杰陈跟平吕龙刚王廷海李晓艳王宗宝常晓昕孙利民康宏敏
Owner PETROCHINA CO LTD
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