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Preparation method of sulfuration-type hydrogenation catalyst

A hydrogenation catalyst and vulcanization-type technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problem of difficult formation of highly active Co-Mo-S or Ni-Mo-S phases , It is not conducive to large-scale industrial production, and the preparation process is cumbersome, etc., to prevent easy overheating, improve intrinsic activity, and facilitate diffusion

Active Publication Date: 2014-05-21
CHINA PETROLEUM & CHEM CORP +1
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  • Claims
  • Application Information

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Problems solved by technology

The patent adopts a two-step method to prepare the catalyst, first forming a molybdenum disulfide phase, and secondary sulfurization after loading metal nickel is not easy to form a highly active Co-Mo-S or Ni-Mo-S phase, and part of the metal nickel is formed without hydrogenation Active nickel sulfide phase, resulting in waste of metallic nickel
The two-step roasting preparation process is cumbersome and economical, which is not conducive to large-scale industrial production

Method used

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  • Preparation method of sulfuration-type hydrogenation catalyst
  • Preparation method of sulfuration-type hydrogenation catalyst
  • Preparation method of sulfuration-type hydrogenation catalyst

Examples

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preparation example Construction

[0026] 1. Preparation of catalyst carrier: Prepare catalyst carrier precursor by conventional method, mix carrier precursor with ammonium thiosulfate, auxiliary agent, molding aid, extrude on extruder, and dry to make catalyst carrier. Drying can be carried out in air or under inert gas. The drying conditions are: 50~148℃ for 1~10h;

[0027] 2. Preparation of sulfurized catalyst

[0028] Prepare the impregnating solution with the required concentration and composition of the active metal to impregnate the carrier, and then dry. The drying condition is: 50-150°C for 1-10 hours, or it can be air-dried. The heat treatment is carried out under an inert atmosphere. The treatment temperature is 180-600° C., and the treatment time is 2-15 hours. Heat treatment is preferably performed in stages, as follows: constant temperature treatment at 180-250°C for 0-5 hours, then constant temperature treatment at 260-350°C for 1-5 hours, and finally constant temperature treatment at 360-600°...

Embodiment 1

[0032] Embodiment 1 Preparation of sulfurized catalyst A

[0033] Take by weighing 900g of pseudo-boehmite (produced by Shandong Aluminum Oxidation Plant, dry basis is 73wt%), 19g of kale powder, 32g of citric acid, 54ml of hexene, 48ml of nitric acid (30% by weight), silica gel (containing Silicon dioxide 30%) 159ml, ammonium thiosulfate solution 250ml (sulfur 60g / 100ml) mixed evenly, extruded into 1.2mm clover strips on the extruder, dried at 120°C for 3 hours in a blast drying oven, that is, Desired Catalyst Support A.

[0034] Take a solution containing ammonium molybdate and nickel nitrate (containing molybdenum oxide 30g / 100ml, containing nickel oxide 5g / 100ml) impregnated carrier A, dried at 120°C for 3 hours, and then heat-treated under nitrogen protection, first raised to 200°C, constant temperature After 2 hours, the temperature was raised to 280°C and kept at a constant temperature for 1 hour, and finally the temperature was raised to 450°C and kept at a constant t...

Embodiment 2

[0035] Embodiment 2 Preparation of sulfurized catalyst B

[0036] Same as Example 1, except that the auxiliary agent is changed to 100ml of coker gasoline (the content of unsaturated hydrocarbon is 49.8v%). The TEM results of the catalyst are shown in figure 2 .

[0037]

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Abstract

The invention discloses a preparation method of a sulfuration-type hydrogenation catalyst. The preparation method is as follows: using a carrier precursor and ammonium thiosulfate and an auxiliary agent for kneading, molding and drying, loading a hydrogenation active metal component, and then performing heat treatment to obtain the sulfuration-type hydrogenation catalyst. The method is simple in preparation process and low in cost. The prepared sulfuration-type hydrogenation catalyst is good in sulfuration effect and high in hydrogenation activity.

Description

technical field [0001] The invention relates to a preparation method of a sulfurized hydrogenation catalyst. Background technique [0002] Conventional hydrogenation catalysts are in an oxidized state, but the active substances are in a sulfurized state in actual use, so they need to be sulfurized in the reactor before use. This not only increases the production cost, but also the vulcanization process is likely to cause pollution to people and the environment, so researchers from all over the world are actively seeking solutions. The current research mainly focuses on two aspects: one is presulfurization outside the device, and the other is the direct preparation of sulfurized catalysts. External presulfurization refers to the introduction of vulcanizing agent into the pores of the oxidized catalyst by sublimation, melting or impregnation, and then the catalyst is partially presulfurized by heating treatment in the presence of inert gas, and finally the catalyst is loaded ...

Claims

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Application Information

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IPC IPC(8): B01J27/051C10G45/08
Inventor 徐黎明高玉兰彭绍忠
Owner CHINA PETROLEUM & CHEM CORP
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