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 to form highly active Co-Mo-S or Ni-Mo-S phase , It is not conducive to large-scale industrial production, and the preparation process is cumbersome, so as to prevent easy overheating, improve distribution, and facilitate diffusion

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

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preparation example Construction

[0027] 1. Preparation of catalyst carrier: Prepare catalyst carrier precursor by conventional method, mix carrier precursor with organic sulfide, 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: 50~280℃ for 1~10h;

[0028] 2. Preparation of sulfurized catalyst

[0029]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: 50-280°C for 1-10 hours, or it can be air-dried. The heat treatment is performed in the presence of at least one of inert gas and hydrogen. The treatment temperature is 200-600°C, and the treatment time is 2-15 hours. The heat treatment is preferably performed in stages, as follows: 0-5 hours at 200-280°C, and then 1-5 hours at 290-350°C. hours, and finally at a constant temperature of 360-600°C for 1-5 hours.

[0030] Method 2: ...

Embodiment 1

[0033] Embodiment 1 Preparation of sulfurized catalyst A

[0034] Weigh 900g of pseudo-boehmite (produced by Shandong Alumina Plant, 73wt% on a dry basis), 19g of scallop powder, 120ml of dimethyl disulfide, 32g of citric acid, 54ml of hexene, nitric acid (weight concentration 30%) 48ml, silica gel (containing silicon dioxide 30% by weight) 159ml, deionized water 100ml mix evenly, extrude into 1.2mm clover strips on the extruder, dry 3 hours at 80 ℃ in the forced air drying oven, obtain the final product Catalyst carrier A is required.

[0035] Take a solution containing ammonium molybdate and nickel nitrate (containing molybdenum oxide 30g / 100ml, nickel oxide 5g / 100ml) impregnated with carrier A, dried at 80°C for 3 hours, and then heat-treated under nitrogen protection. First, the temperature was raised to 200°C and kept constant After 2 hours, then raise the temperature to 320°C, keep the temperature constant for 1 hour, and finally raise the temperature to 450°C and keep ...

Embodiment 2

[0036] Embodiment 2 Preparation of sulfurized catalyst B

[0037] Same as Example 1, except that 100ml of catalytic gasoline (the content of unsaturated hydrocarbons is 49.8v%) is added as an auxiliary agent. The TEM results of the catalyst are shown in figure 2 .

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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 an organic sulfide 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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Patent Type & Authority Applications(China)
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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