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A hydrogenation protecting agent and preparation method thereof

Active Publication Date: 2019-06-11
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 hydrogenation protecting agent and preparation method thereof
  • A hydrogenation protecting agent and preparation method thereof
  • A hydrogenation protecting agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] The preparation of embodiment 1 catalyst carrier

[0051] (1) Preparation of carrier A-1

[0052] Alumina-silica honeycomb ceramics are taken, with a porosity of 5% and an average pore diameter of 2.5 μm. Immerse in boric acid solution, dry at 120°C for 4 hours, and bake at 600°C for 3 hours to obtain carrier A-1, which contains 2wt% boron oxide and 15wt% silicon oxide.

[0053] (2) Preparation of carrier A-2

[0054] Alumina-silica honeycomb ceramics are used, with a porosity of 30% and an average pore diameter of 1.5 μm. Immerse in boric acid solution, dry at 120°C for 4 hours, and bake at 600°C for 3 hours to obtain carrier A-2, which contains 3wt% boron oxide and 12wt% silicon oxide.

Embodiment 2

[0055] Example 2 Preparation of hydrogenation protecting agent B

[0056] Weigh 6.0 g of ammonium molybdate, 4.6 g of nickel nitrate, and 15 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, the sample was put into a blast drying oven for the first low-temperature heat treatment. The conditions for the first low-temperature heat treatment were: the temperature was raised to 80°C at a rate of 3°C / min, and the temperature was kept constant for 3 hours. Dissolve 6.0 g of 2,4,6-trimercapto-s-triazine triammonium salt in 50 mL of water to obtain impregnating solution II, spray the first low-temperature heat-treated sample with impregnating solution II, and then perform the second heat treatment. Low-temperature heat treatment conditions are: at 80°C, water vapor is 50% of the total volume,...

Embodiment 3

[0057] Example 3 Preparation of hydrogenation protecting agent C

[0058] Take 4.9g of molybdenum oxide, 2g of basic nickel carbonate, 0.5mL of phosphoric acid, and 50mL of deionized water and boil for 1 hour to obtain impregnation solution I. Measure the impregnation solution I according to the water absorption rate of 100mL / 100g and spray the carrier A-2. After the spraying is completed, put the sample into the blast drying oven for the first low-temperature heat treatment. The conditions for the first low-temperature heat treatment are: raise the temperature to 80°C at a rate of 3°C / min, and hold the temperature for 3 hours to obtain the first low-temperature heat treatment. For the sample, weigh 8.3g of 2,4-dimercapto-s-triazine diammonium salt and dissolve it in 50mL of water to obtain impregnation solution II. Spray and impregnate the first low-temperature heat treatment sample with impregnation solution II, and then perform the second low-temperature heat treatment , th...

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Abstract

The invention discloses a hydrogenation protection agent and a preparation method thereof. The hydrogenation protection agent comprises a hydrogenation active metal component and a ceramic carrier, and also comprises an organic compound. The protection agent does not need a generation reaction of hydrogen sulfide or a sulfuration reaction of hydrogen sulfide and the active metal in the starting sulfuration process, so the problem of too fast temperature rising in the catalyst sulfuration process is solved, and the starting time is greatly shortened; and the catalyst has the advantages of full sulfuration, good metal dispersion, very high metal removal activity and very strong metal accommodating ability.

Description

technical field [0001] The invention relates to a preparation method of a hydrogenation catalyst, in particular to a hydrogenation protecting agent and a preparation method thereof. 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 deposit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28B01J31/02C10G45/06
CPCB01J31/0244B01J31/28C10G45/06C10G2300/205C10G2300/206C10G2300/70
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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