Process improvement method of vulcanized hydrogenation refining catalyst

A technology for hydrorefining and process improvement, applied in the field of catalysis, can solve the problems of flammability, long process route for catalyst preparation, long vulcanization time, etc., to inhibit the generation of Mo-O-Al bonds, avoid the decrease of active surface area, and reduce the activity of the catalyst. The effect of high metal utilization

Active Publication Date: 2015-05-27
CHINA NAT OFFSHORE OIL CORP +2
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Problems solved by technology

The in-vessel sulfidation method is to put the oxidized catalyst into the hydrogenation reactor, and pass hydrogen and sulfidation agent into the reactor during the heating process for pre-sulfurization. The disadvantage of this method is that it needs special pre-sulfurization equipment, The time is long, the cost of vulcanization is high, the vulcanization agent is highly toxic and flammable, and it is easy to cause pollution t

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  • Process improvement method of vulcanized hydrogenation refining catalyst
  • Process improvement method of vulcanized hydrogenation refining catalyst

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preparation example Construction

[0032] The preparation method of the vulcanized hydrofining catalyst of the present invention is to impregnate the macroporous alumina powder with an impregnating solution containing active metals, and after the in-situ crystallization reaction in a closed container, add a binder and knead, after forming and drying, in an inert gas Roasting under the protection of sulfide type hydrorefining catalyst.

[0033] In the preparation process of the sulfide-type hydrofining catalyst of the present invention, the impregnation method is a conventional method in the field, and the required metal salt, vulcanizing agent, organic complexing agent and dispersant are mixed, stirred and dissolved, and prepared into a clarified product with a suitable pH value. solution, and then impregnated by means of saturated impregnation or excess impregnation.

[0034] The specific preparation method of sulfurized hydrorefining catalyst of the present invention is as follows:

[0035] 1. Configuration ...

Embodiment 1

[0038] The preparation of embodiment 1 sulfurized catalyst A

[0039] Dissolve nickel nitrate, ammonium molybdate and aminotriacetic acid in water to obtain a transparent solution, add polyethylene glycol-400 and thioacetamide in turn, mix and stir to dissolve to form a clear solution, the concentration of polyethylene glycol-400 in the solution The concentration of nickel and molybdenum (calculated as oxide) is 4.5 and 26.0g / 100ml respectively.

[0040] Take 100ml of the mixed solution and spray and soak 100g of macroporous alumina powder (macroporous pseudo-boehmite produced by Shandong Aluminum Company, 68% by weight on a dry basis), in-situ crystallization reaction at 75°C in a closed reaction kettle After 5h, dry in air to loose powder; then add 20g aluminum sol (solid content is 30% by weight), knead in kneader for 30min, then extrude into 1.5mm clover strips on extruder, 130 ℃ air Dry in medium for 8 hours, and finally bake at 480°C for 3 hours under the protection of ...

Embodiment 2

[0041] The preparation of embodiment 2 sulfurized catalyst B

[0042] Dissolve nickel nitrate, ammonium molybdate, ammonium tungstate and amino trimethylene phosphonic acid in water to obtain a transparent solution, add fatty acid polyoxyethylene ester and ammonium thiosulfate in sequence, mix and stir to dissolve to form a clear solution, and the fatty acid polyoxyethylene in the solution The concentration of oxyethylene ester was 2.8g / 100ml, and the concentrations of nickel, molybdenum and tungsten (calculated as oxides) were 4.5, 8 and 18.0g / 100ml, respectively.

[0043] Take 100ml of the mixed solution and spray and soak 100g of macroporous alumina powder (macroporous pseudo-boehmite produced by Shandong Aluminum Company, 68% by weight on a dry basis), in-situ crystallization reaction at 50°C in a closed reaction kettle After 6h, dry in air to loose powder; then add 10g aluminum sol and 10g silica sol (solid content is 30% by weight), knead in kneader for 30min, then extru...

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Abstract

The invention relates to a process improvement method of a vulcanized hydrogenation refining catalyst. The process improvement method is characterized by comprising the following steps: soaking macroporous alumina powder by adopting a dipping solution containing active metal, carrying out the in-situ crystallization, adding the binder, mixing the binder, carrying out the forming and drying, and then carrying out the roasting under the protection of inert gas to obtain the vulcanized hydrogenation refining catalyst. The method is characterized in that the dipping solution contains an inorganic salt precursor of active metal ammonium molybdate and/or ammonium tungstate and Ni and/or Co and also contains an organic vulcanizing agent, a complexing agent, a dispersing agent and the binder; the in-situ crystallization reaction is carried out in a closed vessel after the dipping solution soaks the macroporous alumina powder to prepare the vulcanized catalyst in one step. The method is simple in procedures, low in cost and uniform in dispersion of active metal.

Description

technical field [0001] The invention relates to the technical field of catalysis, in particular to a method for improving the process of a sulfurized hydrorefining catalyst. Specifically, it relates to a process for preparing a sulfurized hydrorefining catalyst by using a conventional active metal salt precursor in one step. Background technique [0002] Petroleum fraction hydrogenation process is the key technology for the production of clean oil products, among which, high-performance hydrotreating catalyst is the key to hydrogenation technology. [0003] Traditional petroleum distillate hydrogenation catalysts are prepared by loading active components such as cobalt, nickel, tungsten and molybdenum on porous carrier materials to prepare supported solid catalysts. Among them, the active components such as cobalt, nickel, tungsten and molybdenum exist in the form of oxides, but in actual use, a sulfurizing agent is used to convert the active components on the petroleum dis...

Claims

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Application Information

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IPC IPC(8): B01J23/883B01J23/888
Inventor 于海斌张景成彭雪峰南军耿姗臧甲忠朱金剑张尚强宋国良肖寒张玉婷张国辉李晓云隋芝宇李佳
Owner CHINA NAT OFFSHORE OIL CORP
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