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A kind of start-up method of hydrogenation catalyst

A hydrogenation catalyst and hydrogenation activity technology, which is applied in the fields of start-up, chemical instruments and methods, catalyst regeneration/reactivation, etc. of hydroprocessing operations, and can solve metal waste, shorten start-up time, and poor dispersion of active metals, etc. problems, to achieve the effect of increasing the initial vulcanization temperature, shortening the start-up time, and good metal dispersion

Active Publication Date: 2019-05-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to avoid excessive temperature rise, the vulcanization process heats up slowly, but this will cause the catalyst vulcanization time to be too long, which is not conducive to shortening the start-up time
Furthermore, both the existing internal presulfurization and external presulfurization will cause insufficient vulcanization of the active metal component in the hydrogenation catalyst, poor dispersion of the active metal, and the inability of the active metal component to fully play its role, resulting in metal waste

Method used

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  • A kind of start-up method of hydrogenation catalyst
  • A kind of start-up method of hydrogenation catalyst
  • A kind of start-up method of hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The preparation of embodiment 1 catalyst carrier

[0042] (1) Preparation of carrier A-1

[0043] Weigh 900g of macroporous pseudoboehmite (73wt% on a dry basis), 19g of scallop powder, 32g of citric acid, 48mL of nitric acid (30wt%), 159mL of silica gel (containing 30wt% of silicon dioxide), polystyrene and Mix 20g each of polyethylene glycol 2000 and 250mL deionized water evenly, extrude into 1.2mm clover strips on an extruder, dry at 120°C for 4 hours, and roast at 600°C for 3 hours to obtain carrier A-1, and the pore volume of carrier A-1 0.7cm 3 / g, the average pore diameter is 35.6nm, and the strength is 176N / cm.

[0044] (2) Preparation of carrier A-2

[0045] Weigh 830g of macroporous pseudo-boehmite (73wt% on a dry basis), 19g of scallop powder, 32g of citric acid, 48mL of nitric acid (30wt%), 200mL of silica gel (containing 30wt% of silicon dioxide), and 50g of alumina powder , 20g each of polystyrene and polyethylene glycol 2000, and 250mL of deionized wa...

Embodiment 2

[0047] (1) Preparation of hydrogenation catalyst B

[0048] Weigh 20.6 g of ammonium molybdate, 14.1 g of nickel nitrate, and 30 mL of ammonia water, and mix them with deionized water to 100 mL to obtain impregnating solution I. Measure the impregnation solution I according to the water absorption rate of 100mL / 100g and spray the impregnation carrier A-1. After spraying, heat treatment at low temperature at 80°C for 3 hours. Take 20g of 2,4,6-trimercapto-s-triazine triammonium salt and dissolve it in 50mL of water to obtain impregnation solution II. Spray the sample with impregnation solution II for low-temperature heat treatment, and dry it in the shade in a ventilated place to obtain hydrogenation catalyst B. Main physical properties See Table 1.

[0049] (2) Catalyst start-up method and evaluation

[0050] After introducing nitrogen into the catalyst reactor, adjust the system pressure to 2.0MPa, directly raise the temperature to 260°C at 25°C / h, keep the temperature for...

Embodiment 3

[0052] (1) Preparation of hydrogenation catalyst C

[0053] Weigh 20.6g of ammonium molybdate, 14.1g of nickel nitrate, and 30mL of ammonia water, mix them with deionized water to 100mL, and divide into 60mL and 40mL. Mix 60mL of the solution with deionized water evenly to 100mL to obtain the soaking solution I. Then measure the impregnation solution I according to the water absorption rate of 100mL / 100g and spray the impregnation carrier A-1, and then perform the first low-temperature heat treatment, the first low-temperature heat treatment condition is: 100°C low-temperature heat treatment for 3 hours. Dissolve 50 g of 2,4,6-trimercapto-s-triazine monoammonium salt in 50 mL of water to obtain impregnation solution II, spray the sample with impregnation solution II for the first low-temperature heat treatment, and then conduct the second low-temperature heat treatment, and the second low-temperature heat treatment The conditions are: 120 ℃ low temperature heat treatment for ...

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Abstract

The invention discloses a start working method of a hydrogenation catalyst. The start working method comprises following steps: 1, a sulfuration-type hydrogenation catalyst is delivered into a reactor; 2, an insert gas is introduced into the reactor to replace air in the reactor, and the sulfuration-type hydrogenation catalyst is subjected to sulfuration in the insert gas atmosphere; 3, after sulfuration, the inert gas is replaced by hydrogen gas, the pressure and the temperature in the reactor are adjusted to a reaction pressure and a reaction temperature when gas flow is stable, and a raw material oil is introduced for hydrogenation, wherein the sulfuration-type hydrogenation catalyst comprises a hydrogenation active metal component, a carrier, and an organic compound. In start working sulfuration, the metal on the surface of the hydrogenation catalyst is subjected to in-suit sulfuration directly, generation reaction of hydrogen sulfide and sulfuration reaction of hydrogen sulfide with active metal are not needed, the initial sulfuration temperature in catalyst start working is increased greatly, rapid temperature increasing in catalyst sulfuration is avoided, and start working time is shortened greatly.

Description

technical field [0001] The invention relates to a catalyst start-up method, in particular to a hydrogenation catalyst start-up method. Background technique [0002] Residue is the heaviest fraction of crude oil and contains high concentrations of metals and asphaltenes. The nature of catalyst deactivation is determined by the nature of special raw materials, and the deactivation of residual oil catalyst mainly depends on metal deposition and coke formation. These impurities cover the surface of the catalyst, reducing the number of active centers, or blocking the pores of the catalyst, hindering the utilization of the inner surface, resulting in the decay of the catalyst activity. Metals in residual oil mainly exist in the form of organometallic compounds (such as nickel and vanadium mainly exist in the form of porphyrin compounds and asphaltenes), these metal compounds decompose during the reaction, and heavy metals are deposited on the catalyst to block the catalyst pores ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J35/10B01J38/10C10G49/24C10G47/00C10G45/00
Inventor 徐黎明高玉兰吕振辉张学辉佟佳孙海
Owner CHINA PETROLEUM & CHEM CORP
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