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On-site external vulcanization processing method of hydrogenation catalysts

A hydrogenation catalyst and sulfidation treatment technology, which is applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc. Hydrogen selectivity, reduction of olefin saturation, high desulfurization rate

Inactive Publication Date: 2015-08-19
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In-situ vulcanization or in-situ vulcanization is to put the catalyst in the oxidation state into the hydrogenation reactor, and then pass hydrogen and sulfidation agents (hydrogen sulfide, carbon disulfide, dimethyl disulfide, etc.) into the reactor during the process of continuous heating. Compounds, etc.) for pre-vulcanization, the disadvantages of this method are: high vulcanization cost; vulcanizing agent is flammable, toxic, and easily pollutes the environment; The generated water and hydrogen sulfide can easily cause corrosion of high-pressure reactors and related equipment
In the US patent US5987816, it is proposed to adopt a fluidized bed process, and to use H in a special presulfurization reactor. 2 / H 2 S gas sulfides the hydrogenation catalyst, and then passivates it with oxygen-containing gas or air. However, during the passivation process, sulfate radicals are generated and remain on the catalyst, which affects the service life of the catalyst.
[0011] To sum up, some of the technologies reported in the current professional literature are limited to written reports and theoretical analysis and have not been implemented. Although the other part has been used in industry, it is not conducive to large-scale industrialization due to complex processes and high preparation costs. production and promotion

Method used

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  • On-site external vulcanization processing method of hydrogenation catalysts
  • On-site external vulcanization processing method of hydrogenation catalysts

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1: Preparation of catalyst carrier

[0039] Weigh 100g of aluminum hydroxide powder, add 3g of sesame powder, mix well, use 100ml of 2wt% nitric acid aqueous solution to acidify, after fully kneading into a gel, extrude it into a cylindrical strip with a diameter of 1.6mm on an extruder. And bake in an oven at 100-120°C for 8-12 hours to obtain a dry carrier. Then, it was placed in a muffle furnace and calcined in an air atmosphere at a temperature of 550° C. for 4 hours to obtain a catalyst carrier A.

Embodiment 2

[0040] Example 2: Loading and curing of molybdenum

[0041] Weigh 2.65g of ammonium paramolybdate, add 14ml of distilled water, stir and dissolve to prepare an immersion solution. 20 g of the carrier A prepared in Example 1 was impregnated with this solution and dried in an oven at 120° C. for 6 hours to obtain a Mo-supported catalyst. The dried catalyst is placed in a tube furnace. The furnace is supplied with a sulfur-containing gaseous mixture of hydrogen sulfide and nitrogen with partial pressures of 0.1 atm and 0.9 atm, respectively, and the temperature is increased to 400°C at a temperature rise rate of 40°C / h , Maintain the temperature for 3 hours to sulfide the catalyst to obtain a catalyst B supporting molybdenum.

Embodiment 3

[0042] Example 3: Cobalt loading and presulfurization

[0043] Weigh cobalt nitrate Co (NO 3 ) 2 ·6H 2 2.4 g of O (analytical purity) was dissolved in 14 ml of distilled water, the Mo-loaded catalyst B prepared in Example 2 was impregnated with the solution, and dried in an oven at 120° C. for 6 hours. The dried catalyst is placed in a tube furnace. The furnace is supplied with a sulfur-containing gaseous mixture of hydrogen sulfide and nitrogen with partial pressures of 0.1 atm and 0.9 atm, respectively, and the temperature is increased to 400°C at a temperature rise rate of 40°C / h , Keep the temperature for 3 hours to sulfide the catalyst to obtain a catalyst C loaded with molybdenum and cobalt. MoO of the catalyst 3 The loading of CoO is 9.28% and 2.72%.

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Abstract

The invention discloses an on-site external vulcanization processing method of hydrogenation catalysts. According to the processing method, at least one kind of sulfur compounds are added into the hydrogenation catalysts in atmosphere of inert gas; on-site external vulcanization processing is carried out at the normal pressure; the vulcanization temperature is 200 to 500 DEG C; the vulcanization time is 0.5 to 48 hours. Compared with in-device pre-vulcanized catalysts prepared by a conventional method, the vulcanization hydrogenation catalysts prepared and pre-vulcanized by the method have the advantages that the desulfurization rate of the vulcanization hydrogenation catalysts prepared by the method of the invention is high, and the activity is good. The on-site external vulcanization processing method of the catalysts is suitable for being used in the preparing process of various kinds of distillate oil hydrogenation catalysts.

Description

Technical field [0001] The invention relates to the technical field of hydrogenation catalyst preparation in the field of petrochemical industry, and in particular to an on-site vulcanization treatment method of a hydrogenation catalyst. Background technique [0002] With the deterioration of crude oil worldwide and the increasingly stringent international environmental protection requirements, higher requirements are placed on the quality of fuels. The hydrogenation process of petroleum fractions is currently one of the effective methods for producing clean fuels, among which highly efficient hydrogenation catalysts It is the key technology of this process. Petroleum fraction hydrogenation catalyst is to support active components such as cobalt, molybdenum, nickel, and tungsten on a porous carrier. Adding additives to the catalyst improves the binding force of the active metal and the carrier, thereby increasing the activity and selectivity of the catalyst. Among them, the acti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/20B01J23/882
Inventor 柴永明刘宾刘晨光柳云骐殷长龙赵会吉张孔远赵瑞玉邢金仙
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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