Pre-sulfurizing process of hydrogenation catalyst

A hydrogenation catalyst and pre-sulfiding technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high price and cumbersome preparation, and achieve low price, simple operation, and avoidance of on-site The effect of pollution

Inactive Publication Date: 2007-09-26
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, the preparation is more cumbersome and the price is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Composition of commercial nickel-molybdenum catalysts in oxidation state MoO 3 is 24wt%, NiO is 3.8wt%, P is 2.6wt%, and the carrier is γ-Al 2 o 3 , diameter 1.2-1.4mm, length 5-10mm, water absorption 0.5mL / g catalyst. Weigh 5.00 g of the catalyst, carry out stoichiometric calculation according to the transformation of the oxidized metal into a sulfide state, the sulfur addition is 1.3 times the required amount, that is, add 3.7 g of 50 wt % ammonium thiosulfate solution, stir well, soak at room temperature for 4 hours, put Dry in an oven at 90°C for 2 hours to obtain 7.01 g of presulfurized catalyst. Crush the pre-sulfided catalyst into 20-40 mesh for later use.

[0025] 1.40g of the obtained pre-sulfided catalyst (equivalent to 1.00g of catalyst in oxidation state) was loaded into a tubular reactor, under 1MPa hydrogen, from room temperature to 300°C in 140 minutes, kept at 300°C for 40 minutes, and dropped to 260°C in 20 minutes , the hydrogen flow rate is 2L / h. ...

Embodiment 2

[0027] Weigh commercial nickel molybdenum (MoO 3 is 24wt%, NiO is 3.8wt%, P is 2.6wt%, and the carrier is γ-Al 2 o 3 ) catalyzer 10.00g, carry out stoichiometric calculation according to oxidation state metal conversion into vulcanization state, sulfur addition is 1.7 times of requirement, namely add 7.8g, the ammonium thiosulfate solution of 62.4wt%, stir evenly, soak for 8 hours, Put it into an oven and dry it at 100° C. for 1 hour to obtain 15.24 g of presulfided catalyst. Crush the pre-sulfided catalyst into 20-40 mesh for later use.

[0028] 1.52 g of the obtained presulfurized catalyst was loaded into a tubular reactor, under 1 MPa hydrogen, from room temperature to 300 °C in 140 minutes, kept at 300 °C for 40 minutes, and decreased to 260 °C in 20 minutes, with a hydrogen flow rate of 2 L / h. The activated catalyst was fed with 1.5% thiophene dissolved in n-nonane model raw material oil, the reaction pressure was 1MPa, the reaction temperature was 260°C, the hydrogen ...

Embodiment 3

[0030] Weigh commercial oxidation state nickel molybdenum catalyst (MoO 3 is 24wt%, NiO is 3.8wt%, P is 2.6wt%, and the carrier is γ-Al 2 o 3 ) 5.00g, carry out stoichiometric calculation according to the conversion of oxidized metal into sulfurized state, the sulfur addition is 0.8 times of the required amount, that is, add 3.3g35wt% ammonium thiosulfate solution, stir evenly, soak for 8 hours, and dry at room temperature for 24 hours, 6.65 g of presulfided catalyst was obtained. Crush the pre-sulfided catalyst into 20-40 mesh for later use.

[0031] 1.13 g of the obtained presulfided catalyst was packed into a tubular reactor, under 1 MPa hydrogen, from room temperature to 300°C in 140 minutes, kept at 300°C for 40 minutes, and decreased to 260°C in 20 minutes, with a hydrogen flow rate of 2 L / h. The activated catalyst was fed with 1.5% thiophene dissolved in n-nonane model raw material oil, the reaction pressure was 1MPa, the reaction temperature was 260°C, the hydrogen ...

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Abstract

The invention relates to a prevulcanization method of hydrogeneration catalyst. The method makes ammonium thiosulfate be loaded on oxidation state catalyst of ni-mo or ni-w and the load quantity is based on the sulfur in ammonium thiosulfate. According to the stoichiometric method, needed sulfur when molybdenum trioxide or tungten trioxide is reduced and sulfurized into molybdenum dioxide or tungten dioxide is 0.5-2 times of needed sulfur when nickel oxide is transferred to nickel sulfide and 1-2 times is selected optically. The load method is that the oxidation state catalyst of ni-mo or ni-w is dipped into the ammonium thiosulfate solution and it is dipped for 0.5-8 hours. The catalyst after dipped is dried for 1-24 hours under the room temperature to 100deg.C in air with normal pressure. The invention is provided with low price, no pollution, simple operation and short sulfurized time.

Description

technical field [0001] The invention belongs to a method for presulfiding a nickel-molybdenum or nickel-tungsten hydrogenation catalyst. Background technique [0002] Nickel-molybdenum or nickel-tungsten catalysts are commonly used in hydrotreating and / or hydrocracking. A hydrotreating catalyst can be defined as any catalyst that can be applied to catalyze the hydrogenation of hydrocarbon feedstocks, especially the hydrogenation of specific components in feedstocks such as sulfur, nitrogen, and metal organic compounds and unsaturates. A hydrocracking catalyst can be defined as any catalytic component that can be used to crack large molecular weight and complex petroleum-derived molecules to give smaller molecules with concomitant hydrogenation of the molecular components. [0003] The catalyst components used for hydrotreating and / or hydrocracking include metal oxides such as cobalt molybdenum, nickel tungsten and nickel molybdenum supported on supports such as alumina, sil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/20C10G45/08
Inventor 李学宽葛军吕占军王建国
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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