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Preparation method of catalyst of sulfur containing transition metal atomic cluster compound for hydrodesulfurizing

A transition metal, hydrodesulfurization technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., to achieve the effect of small metal particle size, simple and easy-to-obtain reaction raw materials, and high metal dispersion degree

Inactive Publication Date: 2006-06-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the metal atom clusters reported in this patent are non-supported

Method used

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Experimental program
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Effect test

Embodiment 1

[0035] Weigh MoO 3 12.0 g, dissolved in concentrated hydrochloric acid, heated to make MoO 3 All dissolved. This solution is placed in an electrolytic cell for electrolysis. After the electrolysis is complete, transfer the electrolyte solution to a sealed bottle for storage. Take part of the solution and dilute it with distilled water at a volume ratio of 1:10, transfer part of the diluted solution to a three-necked bottle, and inject H 2 S gas, carry out vulcanization treatment, vulcanization for 12 hours, H 2 The flow rate of S gas can be controlled within the range of 60-200ml / min. Add hydrochloric acid solution to the vulcanized product, pass air at 110°C, and carry out vacuum distillation and oxidation until the solution volume is about 250ml. The oxidized product was filtered. A portion of the filtrate was taken and diluted with 1N HCl. Take the diluted product and separate it with a gel chromatographic column. Obtain the cluster core prepared by the present inve...

Embodiment 2

[0037] The prepared cluster core is [Mo 3 S 4 ] 4+ The sulfur-containing transition metal molybdenum cluster compound (A) was concentrated with a resin column, mixed with excess metal nickel powder, and stirred at room temperature for 24 hours until the cluster compound A and the nickel powder reacted completely. This mixture was filtered, and the filtrate was separated with a resin column, and Ni was eluted with 0.5N hydrochloric acid. 2+ , and then wash the resin column with 1N hydrochloric acid to separate cluster A. Obtaining the cluster core prepared by the present invention is [NiMo 3 S 4 ] 4+ Sulfur-containing transition metal molybdenum clusters. This cluster is numbered B.

Embodiment 3

[0039] Weigh 3.0 g Al 2 o 3 , Measure a certain amount of cluster compound A, so that the content of metal molybdenum oxide in the catalyst is 7.5%. Al impregnation under nitrogen protection 2 o 3 Carrier, and the solution was evaporated to dryness with a rotary evaporator at a temperature below 60°C. Obtain the Al prepared by the present invention 2 o 3 Supported sulfur-containing transition metal cluster (A) catalyst. This catalyst number is C.

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PUM

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Abstract

A process for preparing the catalyst containing the S and the atom cluster compound of transition metal (Mo or W) and used for hydrodesulfurizing is disclosed. Said atom cluster compound of Mo or W is prepared from its oxide through electrolyzing in acid solution, sulfurizing, oxidizing, concentrating, separation and chemical reaction. Its advantage is high hydrodesulfurizing performance.

Description

technical field [0001] The invention relates to a preparation method of pure-phase and supported sulfur-containing transition metal clusters (including molybdenum and tungsten atom cluster series). Background technique [0002] In recent decades, due to increasingly stringent environmental regulations and the demand for low-quality feedstock oils, the development of new technologies for the production of clean fuel oils has attracted worldwide attention. The development of new technologies for the preparation of low-sulfur gasoline, diesel, and related heavy petroleum and coal-based liquid fuel hydrotreating catalysts has become a new topic that has attracted worldwide attention. At present, most of the liquid fuel hydrodesulfurization catalysts commonly used in industry are supported molybdenum sulfide (or tungsten) catalysts with additives such as nickel and cobalt. Most of these catalysts use ammonium molybdate or ammonium tungstate as raw material, nickel or cobalt as a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/047B01J27/051B01J37/00C10G45/04
Inventor 李灿孙福侠卢绍芳姚元根卢灿忠魏昭彬
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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